CN107146652B - Copper conductive slurry and preparation method and application thereof - Google Patents
Copper conductive slurry and preparation method and application thereof Download PDFInfo
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- CN107146652B CN107146652B CN201710283245.3A CN201710283245A CN107146652B CN 107146652 B CN107146652 B CN 107146652B CN 201710283245 A CN201710283245 A CN 201710283245A CN 107146652 B CN107146652 B CN 107146652B
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- 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
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- 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
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
Abstract
The invention provides a copper conductive paste which comprises the following raw material components in percentage by mass: 65-90 wt% of micron copper powder coated with a nano copper powder layer; 0.1-5 wt% of a dispersant; 9-34% of a solvent. The copper conductive paste uses the micron copper powder as the main conductive filler, and has the advantages of low price, high stacking density and high electron conduction efficiency; the surface of the micron copper powder is coated with a layer of nano copper, and the nano copper is uniformly dispersed and easy to sinter; the optical sintering is directly carried out after the silk screen printing, the process is simple and the method is suitable for large-scale production; the sintered circuit has low resistance and high bending resistance; by adding the stabilizer into the system, the copper oxide is reduced in the sintering process, so that the content of the copper oxide in the copper wire is reduced, and the conductive wire with low copper oxide content is obtained.
Description
Technical Field
The invention relates to electronic paste, in particular to flash lamp sintering electronic paste based on micron copper coated with nano copper.
Background
The method for preparing the conductive copper paste by adopting the nano copper to replace the conductive silver paste is a hot point direction of current research, and particularly, a copper conductive circuit can be obtained on a heat-sensitive substrate by utilizing a technology of sintering the nano copper paste by using a flash lamp. Flash lamp sintering is a novel electronic slurry sintering technology, which adopts wide-spectrum and high-energy pulsed light to carry out curing sintering on nano material slurry and obtain the physical properties of a printing electronic device. The wide application of the technology for preparing the conducting circuit by using the flash lamp sintering nano copper slurry still has a plurality of defects: 1) the nano particles are easy to oxidize, and the electronic paste is difficult to stably store; the sintering conditions need to be strictly controlled; 2) the adoption of the nano particles causes more contact points in the circuit, which is not beneficial to the preparation of a conductive circuit with low resistivity; 3) the manufacturing cost is high by simply adopting the copper nano particles, and the cost performance advantage is not obvious compared with that of silver powder. And micron copper powder is adopted for sintering, because the melting point of the copper powder is higher, only partial fusion can be realized among particles, the fusion degree is small, the binding force among the particles is weak, and the sintered circuit has poor bending resistance and poor wear resistance.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a flash lamp sintering electronic paste based on micron copper coated with nano copper, which is used for solving the problems of low conductivity and poor bending resistance of the flash lamp sintering electronic paste in the prior art.
To achieve the above objects and other related objects, the present application provides the following technical solutions.
The invention provides copper conductive paste which comprises the following raw material components in percentage by weight:
65-90 wt% of micron copper powder coated with nano copper powder layer
0.1 to 5wt% of a dispersant
9-34% of a solvent.
Preferably, the weight percentage of the micron copper powder coated with the nano copper powder layer is 70-85 wt%. More preferably, the weight percentage of the micron copper powder coated with the nano copper powder layer is 77-82 wt%.
Preferably, the weight percentage of the solvent is 10-30 wt%. More preferably, the weight percentage of the solvent is 14-19 wt%.
Preferably, the weight percentage content of the dispersant is 0.8-2.5 wt%.
Preferably, the weight percentage of the solvent is 14-19 wt%.
The technology of coating the nano-structure on the surface of the micron particle has been studied more, and the nano-copper coated micron copper can be prepared by chemically reducing copper salt on the surface of the micron copper. In Chenqingchun, the text of 'hydrothermal preparation of micron copper powder with special morphology' indicates that D-sorbitol is used as a reducing agent, anhydrous copper sulfate is used as a copper source, and a hydrothermal method is used for synthesizing polyhedral copper powder with submicron particle coating on the surface. Patent application No. 200810025661.4 discloses a micron silver-copper particle containing nano-level surface structure, which is prepared by dispersing silver powder, silver-coated copper powder or silver-copper mixed powder in a solvent, reducing silver salt to nano silver powder by using a reducing compound, depositing the nano silver powder on the surface of a substrate, filtering and drying the substrate to obtain the micron silver-copper particle containing nano-level surface structure. The preparation of the micron copper powder coated by the nano copper powder can be realized by a chemical reduction method, and as one implementation method, the micron copper powder is dispersed in a mixed solution of ethanol and water, stirred at a high speed, copper salt (copper nitrate and copper sulfate) and sodium hydroxide are added according to a molar ratio of 1:2, then an aqueous solution of ascorbic acid with equal molar quantity is dripped, stirred for 30min, hydrazine hydrate is dripped until the solution turns black or dark red, the stirring is stopped, and the micron copper powder coated by the nano copper is obtained by centrifugal separation, washing and filtering by ethanol.
Preferably, the thickness of the nano copper powder layer is 10-300 nm.
Preferably, the raw material components of the copper conductive paste include not more than 5wt% of a binder selected from one or more of acrylic resin, polyurethane, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxyethyl hydroxypropyl cellulose, gelatin, gum arabic, peregal, polyethylene glycol, and polyvinyl alcohol. Preferably, the acrylic resin is water-soluble waterborne acrylic resin, and the polyurethane is water-soluble waterborne polyurethane. More preferably, the raw material components of the copper conductive paste include not more than 2.5 wt% of a binder. More preferably, the raw material components of the copper conductive paste comprise (0.8-2.5) wt% of the binder.
Preferably, the raw material components of the copper conductive paste comprise no more than 3 wt% of a stabilizer, and the stabilizer is one or more of glycolic acid, lactic acid, citric acid, malic acid, glucose, glycine, ascorbic acid, glutaraldehyde and a diamine stabilizer. Preferably, the raw material components of the copper conductive paste comprise 1-2.5 wt% of a stabilizer.
Preferably, the particle size of the micron copper powder is 0.5-3 μm. Preferably, the particle size of the micron copper powder is 0.8-3 μm. The copper powder can be spherical, polyhedral, dendritic, flaky or other irregular shapes, and is preferably a polyhedral-shaped near-spherical copper powder, namely a near-spherical particle with more planar shapes, wherein the particle mainly comprises grains with larger sizes, and the grain development is more perfect.
The dispersant can form organic coating on the surface of the copper powder, so that the oxidation resistance of the copper powder is improved. Preferably, the dispersant is selected from one or more of polyvinylpyrrolidone, cetyltrimethylammonium bromide, polyethylene glycol, monoethanolamine, diethanolamine, triethanolamine, linear alkyl ether, hexylamine, octylamine and 2-amino-2-methyl-1-propanol. .
The solvent may be a single solvent or a mixed solvent of a low boiling point solvent and a high boiling point solvent. Preferably, the boiling point of the solvent is 100-300 ℃. Preferably, the solvent is selected from one or more of water, propylene glycol, isopropanol, diethylene glycol, triethylene glycol, diethylene glycol methyl ether, terpineol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, diethylene glycol, ethylene glycol, glycerol, DBE and DPM.
The invention also provides a preparation method of the copper conductive slurry, which comprises the following steps:
the raw material components are uniformly mixed to obtain slurry, and the slurry is added into a three-roll grinder to be ground and then discharged to obtain the copper conductive slurry.
The invention also discloses application of the copper conductive paste, and the conductive paste is used for forming conductive materials of electrodes of radio frequency identification tags, sensors, printed circuit boards, touch screens, solar cells or plasma display screens.
The invention also discloses a forming method of the conductive circuit, wherein the conductive circuit is obtained by forming a pattern on a heat-sensitive substrate by adopting the copper conductive slurry, drying and flash sintering. Preferably, the pattern is formed on the heat-sensitive substrate such as paper, PET, PC or PI by screen printing, gravure printing, flexographic printing, ink jet printing, dip coating or spray coating. More preferably, the drying temperature is 80-150 ℃. Preferably, the drying time does not exceed 60 min. Preferably, the flash sintering energy is 5-15J/cm2。
The invention also discloses a conducting circuit prepared by the method.
The uniformity of dispersion between the nanoparticles and the microparticles is a big problem, and the nanoparticles are easy to agglomerate due to high surface activity and are difficult to be uniformly dispersed in gaps among the micron copper powder particles in the dispersion process. Meanwhile, the agglomerated part undergoes volume shrinkage in the sintering process, so that larger gaps are formed among the micron copper powder, which is not beneficial to improving the conductive performance of the circuit. Poor dispersion uniformity leads to line density and unstable conductivity.
The technology for preparing the copper conductive slurry by taking the micron copper powder as the main body and simultaneously adding the nano particles is hopeful to combine the advantages of the micron copper powder and the nano particles: the volume of the micron particles is reduced in the sintering process, the internal crystal structure is complete, the electron transmission efficiency is high, the nano particles can fill gaps among the micron particles on one hand, the sintering temperature is low, the fusion and recrystallization are easy, and the micron particles can be tightly connected after sintering, so that a high-conductivity and bending-resistant conductive circuit can be obtained.
The copper conductive paste has the following advantages:
1. micron copper powder is used as a main conductive filler, so that the price is low, the stacking density is high, and the electron conduction efficiency is high;
2. the surface of the micron copper powder is coated with a layer of nano copper, and the nano copper is uniformly dispersed and easy to sinter;
3. the photo-sintering is directly carried out after the printing, the process is simple and the method is suitable for large-scale production.
4. The sintered circuit has low resistance and high bending resistance.
5. By adding the stabilizer into the system, the copper oxide is reduced in the sintering process, so that the content of the copper oxide in the copper wire is reduced, and the conductive wire with low copper oxide content is obtained.
Drawings
Fig. 1 shows a scanning electron microscope picture of micron copper powder coated with a nano copper powder layer.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
Before the present embodiments are further described, it is to be understood that the scope of the invention is not limited to the particular embodiments described below; it is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the respective manufacturers.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In addition to the specific methods, devices, and materials used in the examples, any methods, devices, and materials similar or equivalent to those described in the examples may be used in the practice of the invention in addition to the specific methods, devices, and materials used in the examples, in keeping with the knowledge of one skilled in the art and with the description of the invention.
Example 1
Ethylene glycol ethyl ether, diethylene glycol and glycerol were weighed in an amount of 2.5g and 3.5g, respectively, and 1g was added to a beaker, and then 0.4g of PVP, 1.14g of an aqueous polyurethane emulsion (aqueous dispersion having a resin content of 35 wt%), and 0.5g of ascorbic acid were weighed and stirred with a magnetic stirrer for 60 minutes to obtain a homogeneous solution. Weighing 40g of nano-copper-coated micron copper powder (the micron copper powder with the average particle size of 1um and coated with the nano-copper powder layer), gradually adding the nano-copper-coated micron copper powder into the solution, and stirring the solution simultaneously to finally obtain copper slurry with certain viscosity. And mixing and dispersing the obtained copper slurry on a three-roll grinder for 10min to obtain uniform copper slurry.
Printing copper paste on a PET film by screen printing, wherein the width of a printing line is 1mm, the length of the printing line is 150mm (a coil pattern with the length of 40mm and the width of 7 mm), baking the printing line in an oven at 100 ℃ for 20min, performing flash sintering by using a pulse xenon lamp, the pulse width is 2ms, three pulses are used, and the sintering energy is 7J/cm2The test resistance is 2.2 omega, the equivalent sheet resistance is 14.6m omega/□, and the adhesion of the test sample reaches 5B grade according to the ASTM D3359 standard. Will sampleOne end of the product is fixed, and the other end is bent by 90 degrees and repeated for 10 times, and the resistance is measured to be 3.4 omega.
Comparative example 1
In this embodiment, micron copper powder is selected, which is not coated with a nano copper powder layer.
Ethylene glycol ethyl ether, diethylene glycol and glycerol were weighed in an amount of 2.5g and 3.5g, respectively, and 1g was added to a beaker, and then 0.4g of PVP, 1.14g of an aqueous polyurethane emulsion (aqueous dispersion having a resin content of 35 wt%), and 0.5g of ascorbic acid were weighed and stirred with a magnetic stirrer for 60 minutes to obtain a homogeneous solution. And weighing 40g of micron copper powder (with the average particle size of 1 mu m) which is not coated with the nano copper powder layer, gradually adding the micron copper powder into the solution, and stirring the solution simultaneously to finally obtain copper slurry with certain viscosity. And mixing and dispersing the obtained copper slurry on a three-roll grinder for 10min to obtain uniform copper slurry.
Printing copper paste on a PET film by using a screen printing mode, wherein a printing line is 1mm wide and 150mm long (a coil pattern with the length of 40mm and the width of 7 mm), baking in an oven at 100 ℃ for 20min, performing flash sintering by using a pulse xenon lamp, the pulse width is 2ms, three pulses are used, and the sintering energy is 8J/cm2The test resistance is 3.3 omega, the equivalent sheet resistance is 22m omega/□, and the adhesion of the test sample reaches 5B grade according to the ASTM D3359 standard. One end of the sample is fixed, and the other end is bent by 90 degrees and repeated for 5 times, and the resistance is measured to be 130 omega, and the sample is not conductive when being further bent. As is clear from the above comparison, the circuit of comparative example 1 is inferior in bending resistance.
Example 2
Ethylene glycol ethyl ether, diethylene glycol, 3.5g of glycerol and 3.5g of glycerol are weighed respectively, 1g of the mixture is added into a beaker, then 0.6g of PVP, 2.4g of aqueous polyurethane emulsion (aqueous dispersion with 35 wt% of resin content) and 1.2g of ascorbic acid are weighed, and the mixture is stirred for 60min by a magnetic stirrer to obtain a uniform solution. 50g of nano-copper-coated micron copper powder (with the average particle size of 1um) is weighed and gradually added into the solution, and the solution is stirred simultaneously to finally obtain copper slurry with certain viscosity. And mixing and dispersing the obtained copper slurry on a three-roll grinder for 20min to obtain uniform copper slurry.
The method comprises the steps of printing copper paste on a PET film in a screen printing mode, baking the PET film in an oven at 100 ℃ for 20min, carrying out flash sintering by using a pulse xenon lamp, wherein the printed circuit is 1mm wide and 150mm long (a coil pattern with the length of 40mm and the width of 7 mm), the pulse width is 2ms, three pulses are adopted, the sintering energy is 7J/cm2, the test resistance is 3.5 omega, the equivalent square resistance is 23.3m omega/□, and the adhesive force of a test sample reaches 4B level according to the ASTM D3359 standard. One end of the sample was fixed, and the other end was bent 90 degrees and repeated 10 times, whereby the resistance was measured to be 9.0 Ω.
Example 3
Ethylene glycol monomethyl ether, propylene glycol and glycerol are weighed respectively in an amount of 4g, 4g and 4g, added into a beaker, then PVP 1g, aqueous polyurethane emulsion (aqueous dispersion with 35 wt% resin content) 3g and glucose 2g are weighed, and stirred for 60min by a magnetic stirrer to obtain a uniform solution. 65g of nano copper-coated micron copper powder (with the average particle size of 1 mu m) is weighed and gradually added into the solution, and the solution is stirred simultaneously to finally obtain copper slurry with certain viscosity. And mixing and dispersing the obtained copper slurry on a three-roll grinder for 20min to obtain uniform copper slurry.
Printing copper paste on common copy paper by screen printing, wherein the printed circuit has width of 1mm and length of 150mm (40 mm and 7mm wide coil pattern), baking in oven at 90 deg.C for 30min, and flash sintering with pulse xenon lamp, pulse width of 2ms, two pulses, and sintering energy of 10J/cm2The test resistance is 5.2 omega, the equivalent sheet resistance is 34.6m omega/□, and the adhesion of the test sample reaches 4B grade according to the ASTM D3359 standard. The sample was fixed at one end, bent at the other end by 90 degrees, and repeated 10 times, and the resistance was measured to be 18 Ω.
Example 4
Diethylene glycol monomethyl ether, 6g and 6g of diethylene glycol were weighed respectively and added to a beaker, and then 1.5g of PVP and 0.8g of ascorbic acid were weighed and stirred with a magnetic stirrer for 60min to obtain a homogeneous solution. 50g of copper-nanoparticle-coated micron copper powder (with the average particle size of 1um and a polyhedral approximately spherical structure) is weighed and gradually added into the solution, and the solution is stirred simultaneously to finally obtain copper slurry with certain viscosity. And mixing and dispersing the obtained copper slurry on a three-roll grinder for 20min to obtain uniform copper slurry.
Printing copper paste on common copy paper by screen printing, wherein the printed circuit has width of 1mm and length of 150mm (40 mm and 7mm wide coil pattern), baking in oven at 120 deg.C for 25min, and flash sintering with pulse xenon lampPunching width of 2ms, three pulses and sintering energy of 9J/cm2The test resistance is 3.0 omega, the equivalent square resistance is 20.0m omega/□, and the adhesion of the test sample reaches 5B level according to the standard of ASTM D3359. One end of the sample was fixed, and the other end was bent 90 degrees and repeated 10 times, and the resistance was measured to be 3.8 Ω.
Example 5
Respectively weighing 3g, 3g and 3g of ethylene glycol ethyl ether, diethylene glycol and diethanolamine, adding into a beaker, then weighing 1g of polyvinylpyrrolidone, 1.5g of polyvinyl alcohol and 1g of ascorbic acid, and stirring for 60min by using a magnetic stirrer to obtain a uniform solution. 50g of nano-copper-coated micron copper powder (with the average particle size of 1 mu m) is weighed and gradually added into the solution, and the solution is stirred simultaneously to finally obtain copper slurry with certain viscosity. And mixing and dispersing the obtained copper slurry on a three-roll grinder for 20min to obtain uniform copper slurry.
Printing copper paste on a PET film by screen printing, wherein the width of a printing line is 1mm, the length of the printing line is 150mm (a coil pattern with the length of 40mm and the width of 7 mm), baking the printing line in an oven at 80 ℃ for 40min, carrying out flash sintering by using a pulse xenon lamp, the pulse width is 2ms, two pulses are used, and the sintering energy is 10J/cm2The test resistance is 5.5 omega, the equivalent sheet resistance is 36.6m omega/□, and the adhesion of the test sample reaches 4B grade according to the ASTM D3359 standard. One end of the sample was fixed, and the other end was bent 90 degrees and repeated 10 times, and the resistance was measured to be 13 Ω.
Example 6
Respectively weighing ethylene glycol, diethylene glycol and water 4g, 4g and 4g, adding into a beaker, then weighing gelatin 2.0g, polyethylene glycol 1.5g and ascorbic acid 1.5g, and stirring with a magnetic stirrer for 120min to obtain a uniform solution. 66g of copper nanoparticle-coated micron copper powder (average particle size of 1 micron) is weighed and gradually added into the solution, and the solution is stirred simultaneously to finally obtain copper slurry with certain viscosity. And mixing and dispersing the obtained copper slurry on a three-roll grinder for 10min to obtain uniform copper slurry.
Printing copper paste on common copy paper by screen printing, wherein the printed circuit has width of 1mm and length of 150mm (40 mm and 7mm wide coil pattern), baking in oven at 120 deg.C for 10min, and flash sintering with pulse xenon lamp with pulse width of 2ms, one pulse and sintering energy of 10J/cm2The test resistance was 3.6 omega,the equivalent square resistance is 24.0m omega/□, and the adhesion of the test sample reaches 4B grade according to the standard of ASTM D3359. One end of the sample was fixed, and the other end was bent 90 degrees and repeated 10 times, and the resistance was measured to be 4.2 Ω.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (7)
1. The copper conductive paste is characterized by comprising the following raw material components in percentage by mass:
65-90 wt% of micron copper powder coated with nano copper powder layer
0.1 to 5wt% of a dispersant
9-34% of a solvent;
the raw material components of the copper conductive paste comprise not more than 3 wt% of a stabilizer, wherein the stabilizer is one or more of glycolic acid, lactic acid, citric acid, malic acid, glucose, glycine, ascorbic acid, glutaraldehyde and a diamine stabilizer; the dispersing agent is selected from one or more of polyvinylpyrrolidone, cetyl trimethyl ammonium bromide, polyethylene glycol, monoethanolamine, diethanolamine, triethanolamine, linear alkyl ether, hexylamine, octylamine and 2-amino-2-methyl-1-propanol;
the solvent is one or more selected from water, propylene glycol, isopropanol, diethylene glycol, triethylene glycol, diethylene glycol methyl ether, terpineol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, diethylene glycol, ethylene glycol, glycerol, DBE and DPM.
2. The copper conductive paste according to claim 1, characterized in that: the raw material components of the copper conductive paste comprise no more than 5wt% of a binder, wherein the binder is selected from one or more of acrylic resin, polyurethane, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxyethyl hydroxypropyl cellulose, gelatin, gum arabic, peregal, polyethylene glycol and polyvinyl alcohol.
3. The copper conductive paste according to claim 1, characterized in that: the particle size of the micron copper powder is 0.5-3 mu m.
4. A method for producing the copper conductive paste according to any one of claims 1 to 3, comprising the steps of: the raw material components are uniformly mixed to obtain slurry, and the slurry is added into a three-roll grinder to be ground and then discharged to obtain the copper conductive slurry.
5. A forming method of a conductive circuit is characterized in that: the conductive circuit is obtained by forming a pattern on a heat-sensitive substrate by using the copper conductive paste according to any one of claims 1 to 3, drying and flash sintering.
6. An electrically conductive circuit prepared by the method of claim 5.
7. Use of the copper conductive paste according to any one of claims 1 to 3 for forming an electrode of a radio frequency identification tag, a sensor, a printed circuit board, a touch panel, a solar cell or a plasma display panel.
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| CN109226993A (en) * | 2018-08-30 | 2019-01-18 | 桂林电子科技大学 | A kind of micron of copper-silver paste Heat Conduction Material and preparation method thereof |
| CN111548194A (en) * | 2020-05-29 | 2020-08-18 | 南京凯泰化学科技有限公司 | Preparation method of printed circuit board |
| CN113327721B (en) * | 2021-08-04 | 2021-11-30 | 宁波维柔电子科技有限公司 | Preparation method of low-temperature cured conductive copper paste |
| CN115642000B (en) * | 2022-12-23 | 2023-04-07 | 西北工业大学 | Preparation method of conductive copper paste capable of being subjected to photon sintering |
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| CN101214547A (en) * | 2008-01-07 | 2008-07-09 | 李伟强 | Micrometer silver-copper granule containing nano level surface structure and preparation and application thereof |
| CN103480838A (en) * | 2013-10-16 | 2014-01-01 | 哈尔滨工业大学 | Preparation method of nano silver-coated copper powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101214547A (en) * | 2008-01-07 | 2008-07-09 | 李伟强 | Micrometer silver-copper granule containing nano level surface structure and preparation and application thereof |
| CN103480838A (en) * | 2013-10-16 | 2014-01-01 | 哈尔滨工业大学 | Preparation method of nano silver-coated copper powder |
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