CN101880493B - Method for preparing nano copper conductive ink - Google Patents
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Abstract
The invention discloses a method for preparing nano copper conductive ink, which can be applied in the field of printing electronic technology, in particular ink jet printing technology. The preparation method comprises the following steps of: dissolving copper salt and protective agent into a solvent, heating and stirring the solution, adding a small amount of alkali solution to adjust the pH of the solution to between 7 and 10, dripping a reducing agent into the solution, continuously stirring the solution to react for 30 to 60 minutes, and then cooling the reaction solution to room temperature to obtain nano copper dispersion; performing centrifuging, washing and vacuum drying at room temperature on the nano copper dispersion to obtain nano copper granules; and dispersing the nano copper granules into an organic solvent, and ultrasonically treating the solution to obtain the nano copper conductive ink. The method solves the problems of complex preparation process and long preparation period in the prior art, has the advantages of simple and convenient operation, low production cost, short flow and no harmful waste generation, and realizes the goals of environmental protection and economy; and the prepared nano copper conductive ink has good dispersion property and high stability.
Description
Technical field
The present invention relates to the conductive ink technical field in the printed electronics technology, especially relate to a kind of preparation method of nano-copper conductive ink.
Background technology
The ground such as America and Europe, Japan, Korea S and China Taiwan are rising a novel manufacturing technology-printed electronics or printed electronics circuit engineering at present, are also referred to as additive process.This revolutionary new technology adopts various printing technologies on insulating substrate functional ink directly to be printed to circuit or device, is the manufacturing technology of a kind of versatile and flexible, rapid and convenient, environmental protection and energy saving.The material that present research to this technology mainly concentrates on printing technology and is used for printing, i.e. the research of functional ink.
Spray ink Printing is a kind of printing technology extremely wide, that development is ripe of using in daily life.At present, the printed electronics technology becomes a kind of type material processing means from the initial imaging technique development differentiation of writings and image being transferred on the stock from computer, and spray ink Printing is the core process technology of present printed electronics technology.Than traditional materials processing technology, spray ink Printing has rapid shaping, saves time, cost is low, pollution-free, technique flexibly, adapt to the advantages such as various kinds of substrates and flow process be short, make it all have very wide application prospect and huge marketable value at aspects such as electronics, communication, plane demonstration, the energy and medical treatment.For example adopt inkjet technology, directly print the electronic components such as wire, electric capacity, resistance, inductance, diode, triode and for the production of all-inkjet printed circuit card (PCB); By directly print the electronic circuits such as coupling element, antenna, passive and active component is made passive and active wireless radio frequency identification electronic tag (RFID), Organic Light Emitting Diode (OLED), flexible solar battery and medical material etc. in flexibility or rigidity matrix.
The functional ink that is used for spray ink Printing can be scolder and resin, photosensitive polymer (light-cured resin class), nano metal powder (solution), transparent conductor, semi-conductor and isolator, ferrite, reagent, optical absorption agent (being used for organic materials or solar cell etc.), biomaterial (protein molecule, DNA or cell etc.).Wherein the nano metal ink is the main raw material of printed circuit board (PCB)/radio frequency identification electronic label.
It is reported, Korea S inkTec company, Finland VTT research centre, the mechanisms such as Japanese NRI research centre have prepared the nano metal ink of comparative maturity, wherein major part all is based on the jet conductive ink of nanometer silver, and the achievement in research of other conducting metal ink discloses also fewer.But silver is as electro-conductive material, under relatively high temperature and moist environment ion migration occurs easily, and selling at exorbitant prices, the application that these problems have limited silver at the circuit such as PCB and device is a large amount of in producing.Compare with silver, copper is metal the most frequently used in the electronic industry, and its electric conductivity and silver are more or less the same, but its low price only is 1/10th of silver.So people wish that always copper as the surrogate of silver, becomes the main product in the nano metal conductive ink.
Chinese invention patent application prospectus CN200810201967.0 discloses the preparation method of the nano-copper conductive ink that a kind of spray ink Printing uses, it is mantoquita that the method is selected high-purity copper sulfate, sodium hypophosphite is reductive agent, add the organic phase solvent glycol ether (DE gram) of tensio-active agent LD and polyethylene of dispersing agent pyrrolidone (PVP), be heated to 120～160 ℃ and obtain nano copper colloid solution, again by electrodialysis removal of impurities and the concentrated nano-copper conductive ink that obtains of underpressure distillation.The method Heating temperature is high, needs electrodialysis and underpressure distillation operation, thereby complicated process of preparation, and preparation cycle is long.Chinese invention patent application prospectus CN20910054884.8 discloses a kind of preparation method of nano-copper conductive ink, although the method reaction conditions is relatively gentleer: temperature of reaction is 30～100 ℃, has adopted equally electrodialysis and underpressure distillation operation.
Summary of the invention
The technical problem to be solved in the present invention is for the deficiencies in the prior art, and a kind of preparation method of nano-copper conductive ink is provided, and the processing unit of the method is simple, easy to operate, can prepare good dispersity, stable high nano-copper conductive ink.
The present invention solves the problems of the technologies described above the technical scheme that adopts: a kind of preparation method of nano-copper conductive ink comprises the steps:
Step 1: mantoquita and protective material are dissolved in the solvent, are warming up to 30～80 ℃, stir, adding an amount of basic solution adjusting pH value is 7～10, then splashes into reductive agent, continues stirring reaction after 30～60 minutes, is cooled to room temperature, obtains the Nanometer Copper dispersion liquid;
Step 2: the Nanometer Copper dispersion liquid that step 1 is obtained carries out centrifugal, carrying out washing treatment, and then at room temperature vacuum-drying obtains nano copper particle;
Step 3: the nano copper particle that step 2 is obtained is distributed in the organic solvent, and supersound process obtains nano-copper conductive ink.
Wherein, a kind of preferred implementation of above-mentioned steps 2 is: the Nanometer Copper dispersion liquid that step 1 is obtained is in centrifugal treating under 8000～10000 rev/mins the rotating speed after 10～30 minutes, with deionized water and absolute ethanol washing, then at room temperature vacuum-drying is 1～3 hour, obtains nano copper particle.
Among the preparation method of a kind of nano-copper conductive ink of the present invention, organic solvent can be one or more the mixture in butoxy ethyl ester, propylene glycol monomethyl ether acetate, diethylene glycol ether acetic ester, butyl glycol ether, ethylene glycol ether, diethylene glycol monobutyl ether, dibutyl ethylene glycol ether, diethylene glycol diethyl ether, triglyme, triglycol monobutyl ether, triglycol list ether, pimelinketone, hexalin, Terpineol 350, isobutyl ester and the gamma-butyrolactone.
Mantoquita can be at least a in copper sulfate, cupric nitrate, neutralized verdigris, cupric chloride, lauric acid copper and the succsinic acid copper.
Reductive agent can be at least a in sodium hypophosphite, sodium borohydride, xitix, formaldehyde, glucose and the hydrazine hydrate.
Protective material can be small molecules protective material or macromolecule dispersant.Wherein, the small molecules protective material can be at least a in alkyl sulfhydryl, alkyl acid, alkylamine, alkylphosphonic acid carboxylic acid, linear alkyl ether, the micromolecular compound that contains ring texture and their ionic compound; Macromolecule dispersant can be at least a in polyvinyl alcohol, polyoxyethylene glycol, polyvinylpyrrolidone, polyacrylic acid, polymeric amide, polyaniline, Polythiophene, polyethers, urethane, Zelan 338, gelatin, the Sudan Gum-arabic.
Solvent can be one or more the combination in deionized water, ethanol, ethylene glycol, Virahol, glycol ether, the glycerol.
The above-mentioned former dose of mol ratio with mantoquita is 1: 1～5: 1; The mol ratio of protective material and mantoquita is 0.1: 1～10: 1.
Regulate the nano-copper conductive ink that the content that obtains nano copper particle and organic dissolving can obtain different concns among the preparation method of a kind of nano-copper conductive ink of the present invention, in actual use, the weight percent content of preferred nanometer copper particle is 10%～50%.
Utilize the particle diameter of the nano copper particle in the nano-copper conductive ink that the preparation method of a kind of nano-copper conductive ink of the present invention obtains at 20～70nm, and particle dispersion is good, without obvious agglomeration; In addition, the characteristic peak of nano copper particle is obvious, without the characteristic peak of the second-phase impurity such as other cupric oxide or Red copper oxide; This nano-copper conductive ink placed in air coagulation did not occur in one month.
Adopt the preparation technology of electrodialysis and underpressure distillation operation preparation nano-copper conductive ink to compare the Nanometer Copper dispersion liquid with existing, the preparation method of a kind of nano-copper conductive ink of the present invention has abandoned conventional electrodialysis and underpressure distillation operating procedure, employing is carried out centrifugal, carrying out washing treatment to the Nanometer Copper dispersion liquid and is obtained nano copper particle, is re-dispersed into the preparation technology in the organic solvent after being dried.It is unexpected that this preparation technology changes the person skilled in the art of the present invention, because for person skilled in the art of the present invention, although electrodialysis and underpressure distillation operating procedure complex process, but the first-selected technique of the nano-copper conductive ink that it is the preparation good dispersity, stability is high, and adopt other techniques to can not get good dispersity, stable high nano-copper conductive ink.The inventor explores the preparation method that the preparation technology described in the present invention is simple, cost is low at a large amount of experiment basis just, utilizes this preparation method can obtain good dispersity, stable high nano-copper conductive ink.
Therefore, the preparation method of a kind of nano-copper conductive ink of the present invention has overcome complicated process of preparation, the long problem of preparation cycle that exists among the existing preparation method, have easy and simple to handle, production cost is low, flow process is short, the advantage that produces without bazardous waste, realized the target of environmental protection with economy, the good product dispersibility of the nano-copper conductive ink for preparing, stability height, be applicable to the printed electronics technology, especially the inkjet technology field.
Description of drawings
Fig. 1 is the TEM figure of nano copper particle in the nano-copper conductive ink of embodiment 1;
Fig. 2 is the SEM figure of nano copper particle in the nano-copper conductive ink of embodiment 1;
Fig. 3 is the XRD figure of nano copper particle in the nano-copper conductive ink of embodiment 1.
Embodiment
Embodiment is described in further detail the present invention below in conjunction with accompanying drawing.
Embodiment 1:
With 10 mmole CuCl
2.2H
2O and 2.6 gram polyvinylpyrrolidones (PVP) are dissolved in respectively in 50 ml deionized water, and mix and blend is warming up to 80 ℃, and it is 10 that the adding proper ammonia is regulated its pH value; Slowly drip 5 milliliter 50% hydrazine hydrate solution, continue to stir 60 minutes, be cooled to room temperature, obtain the Nanometer Copper dispersion liquid; With the copper dispersion liquid that obtains under 8000 rev/mins rotating speed centrifugal 15 minutes, use respectively deionized water and absolute ethanol washing twice, then at room temperature vacuum-drying is 2 hours, obtains nano copper particle; Take by weighing 0.4 gram nano copper particle, be dissolved in the 0.6 gram diethylene glycol monobutyl ether, obtain solids content after ultrasonic 15 minutes and be 40% nano-copper conductive ink.
With nano-copper conductive ink sampling obtained above, use transmission electron microscope (TEM) and field emission scanning electron microscope (SEM) are observed the copper particle in this nano-copper conductive ink, use x-ray diffractometer (XRD) that this nano-copper conductive ink is carried out the phase atlas analysis, judge to have or not second-phase impurity, obtain Fig. 1, Fig. 2 and Fig. 3.Can find out that from Fig. 1 and Fig. 2 the nano copper particle particle diameter is at 20～70nm in this nano-copper conductive ink, particle dispersion is good, without obvious agglomeration; Can significantly find out the characteristic peak of copper this nano-copper conductive ink from Fig. 3, wherein without any the characteristic peak of the second-phase impurity such as cupric oxide or Red copper oxide; Nano-copper conductive ink obtained above placed in air coagulation did not occur in one month.
Embodiment 2:
With 10 mmole CuSO
45H
2O and 1.62 gram polyacrylamides are dissolved in respectively in 50 milliliters of ethylene glycol and 50 ml deionized water, and mix and blend is warming up to 80 ℃, and it is 9 that the adding proper ammonia is regulated its pH value; Slowly drip 5 milliliter 50% hydrazine hydrate solution, continue to stir 30 minutes, be cooled to room temperature, obtain the Nanometer Copper dispersion liquid; With the copper dispersion liquid that obtains under 8000 rev/mins rotating speed centrifugal 15 minutes, use respectively deionized water and absolute ethanol washing twice, then at room temperature vacuum-drying is 2 hours, obtains nano copper particle; Take by weighing 0.2 gram nano copper particle, be dissolved in the 0.8 gram butyl glycol ether, obtain solids content after ultrasonic 15 minutes and be 20% nano-copper conductive ink.
Fig. 1, Fig. 2 and Fig. 3 in the TEM figure of this nano-copper conductive ink, SEM figure and the XRD figure similar embodiment 1.Show that the nano copper particle particle diameter is at 20～70nm in this nano-copper conductive ink, particle dispersion is good, without obvious agglomeration; The characteristic peak of copper in this nano-copper conductive ink is wherein without any the characteristic peak of the second-phase impurity such as cupric oxide or Red copper oxide; Nano-copper conductive ink obtained above placed in air coagulation did not occur in one month.
Embodiment 3:
With 10 mmole CuCl
2.2H
2O and 2.6 gram polyvinylpyrrolidones (PVP) are dissolved in respectively in 50 milliliters of glycol ethers, and mix and blend is warming up to 30 ℃, and it is 7 that the adding proper ammonia is regulated its pH value; Slowly drip 5 milliliter 50% hydrazine hydrate solution, continue to stir 60 minutes, be cooled to room temperature, obtain the Nanometer Copper dispersion liquid; With the copper dispersion liquid that obtains under 8000 rev/mins rotating speed centrifugal 20 minutes, use respectively deionized water and absolute ethanol washing twice, then at room temperature vacuum-drying is 3 hours, obtains nano copper particle; Take by weighing 0.3 gram nano copper particle and be dissolved in the 0.7 gram diethylene glycol monobutyl ether, obtain solids content after ultrasonic 15 minutes and be 30% nano-copper conductive ink.
Fig. 1, Fig. 2 and Fig. 3 in the TEM figure of this nano-copper conductive ink, SEM figure and the XRD figure similar embodiment 1.Show that the nano copper particle particle diameter is at 20～70nm in this nano-copper conductive ink, particle dispersion is good, without obvious agglomeration; The characteristic peak of copper in this nano-copper conductive ink is wherein without any the characteristic peak of the second-phase impurity such as cupric oxide or Red copper oxide; Nano-copper conductive ink obtained above placed in air coagulation did not occur in one month.
Embodiment 4:
With 10 mmole CuSO
4.5H
2O and 0.54 gram polyacrylamide are dissolved in respectively in 50 ml deionized water, and mix and blend is warming up to 50 ℃, and it is 8 that the adding proper ammonia is regulated its pH value; Slowly drip 3 milliliter 50% hydrazine hydrate solution, continue to stir 30 minutes, be cooled to room temperature, obtain the Nanometer Copper dispersion liquid; With the copper dispersion liquid that obtains under 8000 rev/mins rotating speed centrifugal 15 minutes, use respectively deionized water and absolute ethanol washing twice, then at room temperature vacuum-drying is 2 hours, obtains nano copper particle; Take by weighing 0.2 gram nano copper particle and be dissolved in the 1.8 gram butyl glycol ethers, obtain solids content after ultrasonic 15 minutes and be 10% nano-copper conductive ink.
Fig. 1, Fig. 2 and Fig. 3 in the TEM figure of this nano-copper conductive ink, SEM figure and the XRD figure similar embodiment 1.Show that the nano copper particle particle diameter is at 20～70nm in this nano-copper conductive ink, particle dispersion is good, without obvious agglomeration; The characteristic peak of copper in this nano-copper conductive ink is wherein without any the characteristic peak of the second-phase impurity such as cupric oxide or Red copper oxide; Nano-copper conductive ink obtained above placed in air coagulation did not occur in one month.
Embodiment 5:
With 10 mmole Cu (NO
3)
2Be dissolved in respectively in 50 ml deionized water and the 50 milliliters of Virahols with 8 milliliters of sulfur alcohols, mix and blend is warming up to 70 ℃, and adding proper ammonia, to regulate its pH value be 10.Slowly drip 5 milliliter 50% hydrazine hydrate solution, continue to stir 60 minutes, be cooled to room temperature, obtain the Nanometer Copper dispersion liquid; With the copper dispersion liquid that obtains under 10000 rev/mins rotating speed centrifugal 15 minutes, use respectively deionized water and absolute ethanol washing twice, then at room temperature vacuum-drying is 2 hours, obtains nano copper particle; Take by weighing 0.3 gram nano copper particle, be dissolved in the 0.7 gram diethylene glycol monobutyl ether, obtain solids content after ultrasonic 15 minutes and be 30% nano-copper conductive ink.
Fig. 1, Fig. 2 and Fig. 3 in the TEM figure of this nano-copper conductive ink, SEM figure and the XRD figure similar embodiment 1.Show that the nano copper particle particle diameter is at 20～70nm in this nano-copper conductive ink, particle dispersion is good, without obvious agglomeration; The characteristic peak of copper in this nano-copper conductive ink is wherein without any the characteristic peak of the second-phase impurity such as cupric oxide or Red copper oxide; Nano-copper conductive ink obtained above placed in air coagulation did not occur in one month.
Embodiment 6:
With 10 mmole Cu (NO
3)
2Be dissolved in respectively in 50 ml deionized water and the 50ml ethylene glycol with 10 milliliters of sulfur alcohols, mix and blend is warming up to 60 ℃, and it is 10 that the adding proper ammonia is regulated its pH value.Slowly drip 5 milliliter 50% hydrazine hydrate solution, continue to stir 60 minutes, be cooled to room temperature, obtain the Nanometer Copper dispersion liquid; With the copper dispersion liquid that obtains under 8000 rev/mins rotating speed centrifugal 30 minutes, use respectively deionized water and absolute ethanol washing twice, then at room temperature vacuum-drying is 2 hours, obtains nano copper particle; Take by weighing 0.4 gram nano copper particle and be dissolved in the 0.6 gram dibutyl ethylene glycol ether, obtain solids content after ultrasonic 15 minutes and be 40% nano-copper conductive ink.
Fig. 1, Fig. 2 and Fig. 3 in the TEM figure of this nano-copper conductive ink, SEM figure and the XRD figure similar embodiment 1.Show that the nano copper particle particle diameter is at 20～70nm in this nano-copper conductive ink, particle dispersion is good, without obvious agglomeration; The characteristic peak of copper in this nano-copper conductive ink is wherein without any the characteristic peak of the second-phase impurity such as cupric oxide or Red copper oxide; Nano-copper conductive ink obtained above placed in air coagulation did not occur in one month.
Embodiment 7:
Substantially the same manner as Example 1, difference is after obtaining nano copper particle, takes by weighing 0.4 gram nano copper particle, is dissolved in the 0.6 gram diethylene glycol diethyl ether, obtains solids content after ultrasonic 15 minutes and be 40% nano-copper conductive ink.
Fig. 1, Fig. 2 and Fig. 3 in the TEM figure of this nano-copper conductive ink, SEM figure and the XRD figure similar embodiment 1.Show that the nano copper particle particle diameter is at 20～70nm in this nano-copper conductive ink, particle dispersion is good, without obvious agglomeration; The characteristic peak of copper in this nano-copper conductive ink is wherein without any the characteristic peak of the second-phase impurity such as cupric oxide or Red copper oxide; Nano-copper conductive ink obtained above placed in air coagulation did not occur in one month.
Embodiment 8:
Substantially the same manner as Example 2, difference is after obtaining nano copper particle, takes by weighing 0.2 gram nano copper particle, is dissolved in the 0.8 gram ethylene glycol ether, obtains solids content after ultrasonic 15 minutes and be 20% nano-copper conductive ink.
Fig. 1, Fig. 2 and Fig. 3 in the TEM figure of this nano-copper conductive ink, SEM figure and the XRD figure similar embodiment 1.Show that the nano copper particle particle diameter is at 20～70nm in this nano-copper conductive ink, particle dispersion is good, without obvious agglomeration; The characteristic peak of copper in this nano-copper conductive ink is wherein without any the characteristic peak of the second-phase impurity such as cupric oxide or Red copper oxide; Nano-copper conductive ink obtained above placed in air coagulation did not occur in one month.
Embodiment 9:
Substantially the same manner as Example 3, difference is after obtaining nano copper particle, takes by weighing 0.3 gram nano copper particle, is dissolved in the 0.7 gram triglyme, obtains solids content after ultrasonic 15 minutes and be 30% nano-copper conductive ink.
Fig. 1, Fig. 2 and Fig. 3 in the TEM figure of this nano-copper conductive ink, SEM figure and the XRD figure similar embodiment 1.Show that the nano copper particle particle diameter is at 20～70nm in this nano-copper conductive ink, particle dispersion is good, without obvious agglomeration; The characteristic peak of copper in this nano-copper conductive ink is wherein without any the characteristic peak of the second-phase impurity such as cupric oxide or Red copper oxide; Nano-copper conductive ink obtained above placed in air coagulation did not occur in one month.
Above-mentioned specific embodiment just is used for content of the present invention is described and does not limit the present invention.Should be appreciated that in the situation that does not deviate from scope of the present invention those skilled in the art is after having read content of the present invention, variation or modification that these specific embodiments are carried out all drop in protection scope of the present invention.
Claims (7)
1. the preparation method of a nano-copper conductive ink is characterized in that: comprise the steps:
Step 1: mantoquita and protective material are dissolved in the solvent, are warming up to 30～80 ℃, stir, adding an amount of basic solution adjusting pH value is 7～10, then splashes into reductive agent, continues stirring reaction after 30～60 minutes, is cooled to room temperature, obtains the Nanometer Copper dispersion liquid; The mol ratio of described reductive agent and mantoquita is 1:1～5:1; The mol ratio of described protective material and mantoquita is 0.1:1～10:1; Described protective material is small molecules protective material or macromolecule dispersant; Described small molecules protective material is at least a in alkyl sulfhydryl and ionic compound, alkyl acid and ionic compound thereof, alkylamine and ionic compound thereof, alkylphosphonic acid carboxylic acid and ionic compound thereof, linear alkyl ether and ionic compound thereof, the micromolecular compound that contains ring texture and the ionic compound thereof; Described macromolecule dispersant is at least a in polyvinyl alcohol, polyoxyethylene glycol, polyvinylpyrrolidone, polyacrylic acid, polymeric amide, polyaniline, Polythiophene, polyethers, urethane, Zelan 338, gelatin, the Sudan Gum-arabic;
Step 2: the Nanometer Copper dispersion liquid that step 1 obtains after 10～30 minutes, is used deionized water and absolute ethanol washing in centrifugal treating under 8000～10000 rev/mins the rotating speed, and then at room temperature vacuum-drying is 1～3 hour, obtains nano copper particle;
Step 3: the nano copper particle that step 2 is obtained is distributed in the organic solvent, and supersound process obtains nano-copper conductive ink.
2. the preparation method of a kind of nano-copper conductive ink according to claim 1 is characterized in that: described organic solvent is one or more the mixture in butoxy ethyl ester, propylene glycol monomethyl ether acetate, diethylene glycol ether acetic ester, butyl glycol ether, ethylene glycol ether, diethylene glycol monobutyl ether, dibutyl ethylene glycol ether, diethylene glycol diethyl ether, triglyme, triglycol monobutyl ether, triglycol list ether, pimelinketone, hexalin, Terpineol 350, isobutyl ester, the gamma-butyrolactone.
3. the preparation method of a kind of nano-copper conductive ink according to claim 1 and 2 is characterized in that: described mantoquita is at least a in copper sulfate, cupric nitrate, neutralized verdigris, cupric chloride, lauric acid copper and the succsinic acid copper.
4. the preparation method of a kind of nano-copper conductive ink according to claim 1 and 2 is characterized in that: described reductive agent is at least a in sodium hypophosphite, sodium borohydride, xitix, formaldehyde, glucose and the hydrazine hydrate.
5. the preparation method of a kind of nano-copper conductive ink according to claim 1 and 2 is characterized in that: described solvent is one or more the combination in deionized water, ethanol, ethylene glycol, Virahol, glycol ether, the glycerol.
6. the preparation method of a kind of nano-copper conductive ink according to claim 1 and 2, it is characterized in that: the weight percent content of copper particle is 10%～50% in the described nano-copper conductive ink.
7. the preparation method of a kind of nano-copper conductive ink according to claim 1 and 2, it is characterized in that: the particle diameter of described nano copper particle is 20～70nm.
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| CN114749656A (en) * | 2020-12-28 | 2022-07-15 | 航天神舟生物科技集团有限公司 | Preparation method of metal nano iron/nano copper particle solution and working solution |
| WO2023132756A1 (en) * | 2022-01-07 | 2023-07-13 | Nairotech Desarrollo E Innovación S.A. | Suspended metal nanoparticle |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101608077A (en) * | 2009-07-16 | 2009-12-23 | 复旦大学 | A kind of preparing nano copper conductive |
| CN101684214A (en) * | 2008-09-26 | 2010-03-31 | 昆山海斯电子有限公司 | Nanoparticle conductive ink and preparation method thereof |
-
2010
- 2010-07-01 CN CN 201010221315 patent/CN101880493B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101684214A (en) * | 2008-09-26 | 2010-03-31 | 昆山海斯电子有限公司 | Nanoparticle conductive ink and preparation method thereof |
| CN101608077A (en) * | 2009-07-16 | 2009-12-23 | 复旦大学 | A kind of preparing nano copper conductive |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018118460A1 (en) * | 2016-12-24 | 2018-06-28 | Electroninks Incorporated | Copper based conductive ink composition and method of making the same |
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