CN113689972A - Preparation method of conductive silver-clad copper paste for flexible circuit - Google Patents
Preparation method of conductive silver-clad copper paste for flexible circuit Download PDFInfo
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- CN113689972A CN113689972A CN202110847958.4A CN202110847958A CN113689972A CN 113689972 A CN113689972 A CN 113689972A CN 202110847958 A CN202110847958 A CN 202110847958A CN 113689972 A CN113689972 A CN 113689972A
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- silver
- copper paste
- conductive silver
- carbon nanotubes
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims description 43
- 229910052802 copper Inorganic materials 0.000 title description 27
- 239000010949 copper Substances 0.000 title description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 51
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 50
- NEIHULKJZQTQKJ-UHFFFAOYSA-N [Cu].[Ag] Chemical compound [Cu].[Ag] NEIHULKJZQTQKJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002002 slurry Substances 0.000 claims abstract description 23
- 238000005452 bending Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 9
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000004433 Thermoplastic polyurethane Substances 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 36
- 229910052709 silver Inorganic materials 0.000 claims description 36
- 239000004332 silver Substances 0.000 claims description 36
- 238000001723 curing Methods 0.000 claims description 6
- 238000009826 distribution Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- 239000002318 adhesion promoter Substances 0.000 claims description 2
- 229920003180 amino resin Polymers 0.000 claims description 2
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical class NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 2
- 230000001788 irregular Effects 0.000 claims description 2
- 238000013035 low temperature curing Methods 0.000 claims description 2
- 239000002048 multi walled nanotube Substances 0.000 claims description 2
- -1 phthalate ester Chemical class 0.000 claims description 2
- 239000002109 single walled nanotube Substances 0.000 claims description 2
- 229920005992 thermoplastic resin Polymers 0.000 claims description 2
- 239000002562 thickening agent Substances 0.000 claims description 2
- 125000004185 ester group Chemical group 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 10
- 239000002131 composite material Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 238000013329 compounding Methods 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 abstract 1
- 238000007639 printing Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000007650 screen-printing Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000002411 thermogravimetry Methods 0.000 description 3
- 239000004642 Polyimide Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 108091006149 Electron carriers Proteins 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- HGAZMNJKRQFZKS-UHFFFAOYSA-N chloroethene;ethenyl acetate Chemical compound ClC=C.CC(=O)OC=C HGAZMNJKRQFZKS-UHFFFAOYSA-N 0.000 description 1
- 238000002788 crimping Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- 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
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- 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
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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)
- Parts Printed On Printed Circuit Boards (AREA)
- Conductive Materials (AREA)
Abstract
The application provides a preparation method of low-temperature conductive silver copper paste for a flexible circuit. The silver copper paste formula comprises: 20-80 wt% of micron/submicron silver-copper powder, 1-20 wt% of thermoplastic polyurethane, 1-20 wt% of curing agent, 10-50 wt% of solvent, 0.1-10 wt% of carbon nano tube, 0.1-20 wt% of auxiliary agent and the like. The formula is mixed according to a certain proportion, and then the uniform composite conductive silver-copper slurry is formed through the processes of double-paddle stirring, three-roller shaft dispersion and the like. Through the compounding mode, the conductive silver-copper paste shows excellent conductive characteristic and bending resistance after being printed and cured on the flexible base material, and can be widely applied to various flexible electronic components.
Description
Technical Field
The application relates to the field of low-temperature conductive paste, in particular to a preparation method and application of low-temperature conductive silver-coated copper paste for screen printing of a flexible circuit.
Background
With the rapid development of the electronic industry, the fields of flexible electronic devices, including OLED displays, flexible sensors, organic solar cells, etc., are gaining popularity and growing rapidly. Advanced electronic material technology is a key technology for flexible electronic devices. The full-printed electronic technology is a method for manufacturing circuits and electronic devices by utilizing the traditional printing technology, and the printing technology is organically combined with an electronic manufacturing process, so that the environment-friendly, efficient and low-cost production of electronic products is realized. The materials used in the full-printed electronic technology mainly comprise electronic paste and various substrates, wherein more and more substrates mainly comprise organic films and have the characteristics of lightness, thinness and flexibility. The conductive paste is of great interest as a key functional material in various electronic products.
The low-temperature conductive slurry is viscous slurry formed by uniformly dispersing micron/nano metal powder in an organic resin phase. Its conductive function is mainly achieved by free electron carriers provided by the metal phase. In addition to the particle size and purity of the metal powder, the choice of the resin carrier also affects the properties of the conductive paste. At present, most of the commonly used resins are epoxy resin and vinyl chloride-vinyl acetate resin, but the cured resins have poor mechanical properties and poor impact resistance, so that polyurethane is selected as a carrier of silver-coated copper paste to enhance the flexibility and bending resistance of the paste after curing.
Carbon Nanotubes (CNTs) are a novel one-dimensional functional nanomaterial, formed by crimping single-or multi-layer graphite flakes, and have excellent mechanical, electrical, and thermal properties. The graphite sheet layer of the carbon nano tube is mainly a C-C covalent bond, has very stable chemical property and strong bonding force, the Young modulus of the graphite sheet layer is as high as 1.0TPa, the tensile strength of the graphite sheet layer can reach 45GPa, and the tensile strength of the graphite sheet layer is 20 times that of high-strength steel. Therefore, carbon nanotubes have great potential in the field of composite materials. The CNT with a certain proportion is added into the prepared silver-coated copper paste, so that the advantages of the silver-coated copper paste and the CNT are hopefully combined, and the conductive property, the bending resistance and the like of the silver-coated copper paste are improved.
Disclosure of Invention
1. The application provides a preparation method and application of low-temperature conductive silver-coated copper paste for a screen printing flexible circuit, the silver-copper paste can be applied to a membrane switch, a keyboard and a flexible sensor, has excellent conductivity and bending resistance, and is bent for 10 times in a positive and negative 180 degrees, and the resistance change rate is less than 300%.
A conductive silver copper paste doped with carbon nanotubes comprises the following components:
20-80 wt% of silver-coated copper powder;
0.1-10 wt% of Carbon Nanotube (CNT);
1-20 wt% of Thermoplastic Polyurethane (TPU);
1-20 wt% of curing agent
10-50 wt% of a solvent;
0.1-20 wt% of an auxiliary agent;
wherein, the components of the slurry are mixed and dispersed in modes of full stirring, three-roller grinding and the like to form uniform slurry.
2. The carbon nanotube doped conductive silver copper paste according to claim 1, wherein: the silver-coated copper powder is in one or more of flake, spherical, dendritic and irregular shapes.
3. The carbon nanotube doped conductive silver-clad copper paste according to claim 1, wherein: the particle size distribution of the silver-coated copper powder is D100.1-2 μm, D501-5 μm and D903-20 μm.
4. The carbon nanotube doped conductive silver-clad copper paste according to claim 1, wherein: the silver content (mass ratio) of the silver-coated copper powder is between 1% and 50%.
5. The carbon nanotube doped conductive silver-clad copper paste according to claim 1, wherein: the carbon nano tube is one or two of a single-wall carbon nano tube and a multi-wall carbon nano tube.
6. The carbon nanotube doped conductive silver-clad copper paste according to claim 1, wherein: the particle size distribution of the carbon nano tube is 2 nm-10 mu m of tube diameter and 100 nm-100 mu m of tube length.
7. The carbon nanotube doped conductive silver-clad copper paste according to claim 1, wherein: the thermoplastic resin includes, but is not limited to, one or more of basf 1170A, bayer 192X, lubol 61083, tabasheer WHT-6232B.
8. The carbon nanotube doped conductive silver-clad copper paste according to claim 1, wherein: the low-temperature curing agent is selected from one or more of modified dicyandiamide, phthalate ester, a silane coupling agent and amino resin.
9. The carbon nanotube doped conductive silver-clad copper paste according to claim 1, wherein: the solvent is ester, ether or alcohol solvent with higher boiling point.
10. The carbon nanotube doped conductive silver-clad copper paste according to claim 1, wherein: the auxiliary agent comprises an adhesion promoter, a thickening agent, a flatting agent, a defoaming agent and the like.
Drawings
FIG. 1: scanning Electron Microscope (SEM) picture of silver-coated copper powder
FIG. 2: energy spectrometer (EDS) element distribution diagram of silver-coated copper powder
FIG. 3: CNT Scanning Electron Microscope (SEM) image
FIG. 4: thermogravimetric analysis data of CNT silver coated copper paste
FIG. 5: CNT silver coated copper paste and printed test pattern
FIG. 6: bending test resistance data
FIG. 7: electron micrographs before and after bending
Detailed Description
In order to illustrate the invention more clearly, the invention is further described below with reference to the accompanying drawings and specific examples, which should not be construed as limiting the scope of the invention.
The preparation method of the carbon nano tube silver-coated copper slurry comprises the following steps: respectively weighing silver-coated copper powder, thermoplastic polyurethane resin, CNT powder, a solvent and an auxiliary agent, adding the silver-coated copper powder, the thermoplastic polyurethane resin, the CNT powder, the solvent and the auxiliary agent into a slurry tank, stirring for 1 hour by using a double-paddle stirrer until the powder is uniform and fully infiltrated, then dispersing the CNT silver-copper slurry composite slurry to the fineness of less than 10 mu m by using a three-roller shaft grinding machine, and collecting to obtain the uniformly dispersed silver-copper slurry.
Example 1
The formula and the preparation process of the silver-copper paste comprise the following steps:
adding 51 wt% of flaky silver-coated copper powder (with silver content of 20%), 8 wt% of thermoplastic polyurethane, 1 wt% of CNT powder, 31 wt% of solvent and 9 wt% of auxiliary agent into a slurry tank, stirring for 10 minutes by using a stainless steel spatula to fully soak the silver-copper powder, stirring for 1 hour by using a slurry stirrer until the mixture is uniform, then grinding the CNT silver-coated copper composite slurry for six times by using a three-roll-shaft grinding machine, and collecting to obtain uniformly dispersed silver-copper slurry.
FIG. 1 is a Scanning Electron Microscope (SEM) image of silver-coated copper powder with the silver powder morphology being flake. Fig. 2 is an Energy Dispersive Spectroscopy (EDS) elemental distribution diagram of silver-coated copper powder with silver uniformly distributed on the surface of the copper. Fig. 3 is a Scanning Electron Microscope (SEM) image of CNTs, which appear as nanowires.
Fig. 4 shows thermogravimetric analysis data of the CNT-silver coated copper paste. Specifically, the temperature rise rate of the thermogravimetry is 2 ℃/min, the temperature is raised from room temperature 25 ℃ to 200 ℃, as shown in fig. 1, 59.78% of mass remains when the silver-copper slurry is further raised to 200 ℃, which indicates that the solid content of the slurry is close to 60%.
The printing was done using a manual screen printing station, 200 mesh stainless steel screen, with the pattern shown in fig. 5 printed on a Polyimide (Polyimide) PI substrate, and then cured in an oven at 120 ℃ for 10 minutes.
And testing the fine line resistance condition of the CNT silver-coated copper paste after printing and curing by using a multimeter. Wherein, the length of the thin line is 5cm, and the line width is 1mm, 2mm and 3mm respectively. Through measurement, the average resistance of the 1mm wire is 2.1 omega, the average resistance of the 2mm wire is 1.4 omega, the average resistance of the 3mm wire is 1.0 omega, and the slurry has good conductivity.
And in addition, the obtained CNT silver-coated copper paste is printed with patterns, and 3mm lines after solidification are selected for carrying out bending resistance test on the CNT silver-coated copper paste. The specific test method is to bend the 3mm silver-copper paste after printing and curing at 180 degrees, and then place a 1000 g weight at the crease and keep for 1 minute. It was then bent in the opposite direction at 180 ° and a 1000 gram weight was placed at the fold again for 1 minute, and this was repeated 10 times. Fig. 6 shows the resistance change after bending for 3 samples. FIG. 7 is a scanning electron microscope image of the surface before and after bending, with no apparent cracks in the surface after bending, suitable for flexible circuit printing and applications.
Example 2
The formula and the preparation process of the CNT silver-coated copper paste comprise the following steps:
adding 60 wt% of silver-coated copper powder, 8 wt% of thermoplastic polyurethane, 0.2 wt% of CNT powder, 25 wt% of solvent and 6.8 wt% of auxiliary agent into the slurry, stirring for 10 minutes by using a stainless steel spatula to fully soak the silver-copper powder, stirring for at least 1 hour by using a double-paddle stirrer until the mixture is uniform, dispersing the CNT silver-coated copper slurry composite slurry for six times by using a three-roll shaft, and collecting to obtain uniformly dispersed conductive slurry. Printing, curing and testing were the same as in example 1.
Claims (10)
1. The preparation method of the conductive silver-copper paste doped with the carbon nano tube can be applied to a film switch, a keyboard and a flexible sensor, has excellent conductivity and bending resistance, and has a resistance change rate of less than 300% after being bent for 10 times in a positive and negative 180 degrees manner;
a conductive silver copper paste doped with carbon nanotubes comprises the following components:
20-80 wt% of silver-coated copper powder;
0.1-10 wt% of Carbon Nanotube (CNT);
1-20 wt% of Thermoplastic Polyurethane (TPU);
1-20 wt% of curing agent
10-50 wt% of a solvent;
0.1-20 wt% of an auxiliary agent;
wherein, the components of the slurry are mixed and dispersed in modes of full stirring, three-roller grinding and the like to form uniform slurry.
2. The method of claim 1, wherein the conductive silver-copper paste doped with carbon nanotubes comprises: the silver-coated copper powder is in one or more of flake, spherical, dendritic and irregular shapes.
3. The method of claim 1, wherein the conductive silver-copper paste doped with carbon nanotubes comprises: the particle size distribution of the silver-coated copper powder is D100.1-2 μm, D501-5 μm and D903-20 μm.
4. The method of claim 1, wherein the conductive silver-copper paste doped with carbon nanotubes comprises: the silver content (mass ratio) of the silver-coated copper powder is between 1% and 50%.
5. The method of claim 1, wherein the conductive silver-copper paste doped with carbon nanotubes comprises: the carbon nano tube is one or two of a single-wall carbon nano tube and a multi-wall carbon nano tube.
6. The method of claim 1, wherein the conductive silver-copper paste doped with carbon nanotubes comprises: the particle size distribution of the carbon nano tube is 2 nm-10 mu m of tube diameter and 100 nm-100 mu m of tube length.
7. The method of claim 1, wherein the conductive silver-copper paste doped with carbon nanotubes comprises: the thermoplastic resin includes, but is not limited to, one or more of basf 1170A, bayer 192X, lubol 61083, tabasheer WHT-6232B.
8. The method of claim 1, wherein the conductive silver-copper paste doped with carbon nanotubes comprises: the low-temperature curing agent is selected from one or more of modified dicyandiamide, phthalate ester, a silane coupling agent and amino resin.
9. The method of claim 1, wherein the conductive silver-copper paste doped with carbon nanotubes comprises: the solvent is ester, ether or alcohol solvent with higher boiling point.
10. The method of claim 1, wherein the conductive silver-copper paste doped with carbon nanotubes comprises: the auxiliary agent comprises an adhesion promoter, a thickening agent, a flatting agent, a defoaming agent and the like.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110847958.4A CN113689972A (en) | 2021-07-27 | 2021-07-27 | Preparation method of conductive silver-clad copper paste for flexible circuit |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110847958.4A CN113689972A (en) | 2021-07-27 | 2021-07-27 | Preparation method of conductive silver-clad copper paste for flexible circuit |
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| CN202110847958.4A Withdrawn CN113689972A (en) | 2021-07-27 | 2021-07-27 | Preparation method of conductive silver-clad copper paste for flexible circuit |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115274213A (en) * | 2022-04-26 | 2022-11-01 | 南京纳纬新材料科技有限公司 | Preparation method of bending-resistant resistance carbon paste |
| CN115458233A (en) * | 2022-09-26 | 2022-12-09 | 苏州思尔维纳米科技有限公司 | Conductive paste, preparation method thereof and electronic device |
| CN117690634A (en) * | 2023-12-13 | 2024-03-12 | 深圳市绚图新材科技有限公司 | Composite conductive paste of carbon network and metal and preparation method thereof |
-
2021
- 2021-07-27 CN CN202110847958.4A patent/CN113689972A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115274213A (en) * | 2022-04-26 | 2022-11-01 | 南京纳纬新材料科技有限公司 | Preparation method of bending-resistant resistance carbon paste |
| CN115458233A (en) * | 2022-09-26 | 2022-12-09 | 苏州思尔维纳米科技有限公司 | Conductive paste, preparation method thereof and electronic device |
| CN115458233B (en) * | 2022-09-26 | 2026-01-30 | 苏州思尔维纳米科技有限公司 | Conductive paste, its preparation method and electronic devices |
| CN117690634A (en) * | 2023-12-13 | 2024-03-12 | 深圳市绚图新材科技有限公司 | Composite conductive paste of carbon network and metal and preparation method thereof |
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Application publication date: 20211123 |