CN103212715B - A kind of copper silver nanoparticle electrocondution slurry and synthetic method thereof - Google Patents
A kind of copper silver nanoparticle electrocondution slurry and synthetic method thereof Download PDFInfo
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- CN103212715B CN103212715B CN201210016798.XA CN201210016798A CN103212715B CN 103212715 B CN103212715 B CN 103212715B CN 201210016798 A CN201210016798 A CN 201210016798A CN 103212715 B CN103212715 B CN 103212715B
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Abstract
The invention discloses a kind of synthetic method of copper silver nanoparticle electrocondution slurry, silver salt is dissolved in the alcohol organic solvent of nitrogenous organic ligand and obtains silver complex solution by the method, silver complex solution is added drop-wise in copper nano particles dispersion liquid, copper can reduce silver ion rapidly, the deposition of silver generated is to the surface of copper nano particles or be dispersed in reactant liquor, is scattered in organic solvent and makes electrocondution slurry.The electrocondution slurry that the inventive method prepares has good oxidative resistance, and sintering temperature is low, is applicable to the substrates such as polyvinyl chloride, polyethylene, polyester, nylon, glass.
Description
Technical field
The present invention relates to the synthesis field of electrocondution slurry, specifically a kind of copper silver nanoparticle electrocondution slurry and synthetic method thereof.
Background technology
Metal conductive paste has a wide range of applications in modern electronics industry field, formed by the microns such as metal gold, silver, copper, nickel or aluminium or nano particle and suitable preparation of reagents, wherein gold and silver are owing to having good stability, and high conductance, and in high-end electrocondution slurry market share leading position, but its price is high; Based on the electrocondution slurry of copper or aluminium, price is lower, but is easy to oxidation due to it, and range of application is not very wide.Recently, based on the electrocondution slurry of silver-colored copper-clad, make some progress, copper silver is carried out coated, the stability of electrocondution slurry can be added like this, additionally reduce the consumption of silver in electrocondution slurry, reduce the cost of electrocondution slurry, as patent US4652465 adopts ammonium carbonate to be additive, silver ion is by the copper reduction of acid activation, silver-colored at micron-sized copper surface deposition last layer; Patent US5178909 utilizes reducing agent reduction silver ion, adds nitrogenous chelating reagent, promotes silver deposition on copper surfaces; Patent US5945158 adopts amine sulfate and ammonia spirit to activate micron-sized copper particle, and successively add reducing agent and silver salt ammonia spirit, silver salt reduces by reducing agent, and deposition of silver to copper micron particles on the surface; Patent US20070212562 adopts primary amine to be solvent, obtains copper nano particles, then directly in system, add silver salt solution with reducing agent reduction cupric, excessive reducing agent by silver ion reduction, at the deposited on silicon silver of nano copper particle; Patent US20110183128 adopts polymer to be stabilizing agent, trap is reducing agent, reduction cupric obtains copper nano particles, copper nano particles aldehydes reagent processes, obtain without trap copper nano particles, in system, add silver salt solution afterwards, silver reduces by copper nano particles, obtains copper silver core-shell nanoparticles.Although these above methods have made some progress, the problems such as the method that there is synthesis is complicated, sintering temperature is high and conductance is on the low side.
Summary of the invention
The object of the invention is the preparation method that a kind of copper silver nanoparticle electrocondution slurry is provided for the deficiencies in the prior art.Silver salt is dissolved in the solution of nitrogenous organic ligand by the method prepares silver complex solution, silver complex solution is added drop-wise in copper nano particles dispersion liquid, copper is by silver ion reduction, generate deposition of silver to copper nano particles on the surface or part be dispersed in reactant liquor, copper silver composite nanometer particle is separated, and is scattered in obtained copper silver nanoparticle electrocondution slurry in organic solvent.
A kind of copper silver nanoparticle electrocondution slurry synthetic method provided by the invention, comprises the steps:
(1) silver complex solution is prepared:
Silver salt is dissolved in the alcohol organic solvent containing nitrogen machine part and prepares silver complex solution;
(2) copper nano particles dispersion liquid is prepared:
Under nitrogen atmosphere, copper nano particles is scattered in organic solvent obtains copper nano particles dispersion liquid;
(3) copper silver nanoparticle electrocondution slurry is prepared:
At room temperature under an n 2 atmosphere, be added drop-wise in described copper nano particles dispersion liquid by described silver complex solution and react, reaction product isolated obtains copper silver composite nanometer particle, and is scattered in organic solvent and obtains copper silver nanoparticle electrocondution slurry.
Wherein, the molar ratio of described silver salt and nitrogenous organic ligand is 1:1-10; The mass percent solubility of described silver salt is 4-55%.
Wherein, described copper nano particles can directly be bought from market or adopt chemical reduction method to synthesize and obtain, as adopted document Nanotechnology 19 (2008) 415604, Journal of Colloid and Interface Science 277 (2004) 100 – 103, the method synthesis that Journal of Nanoparticle Research 13 (2011) 127-138 reports, be particularly suitable for adopting the synthesis of the method disclosed in Chinese patent (application number 201110355856.7) to obtain, be characterized in that copper nano particles adopts the synthetic method of semi-solid phase heating using microwave to obtain.In the present invention, the synthetic method of copper nano particles is not limited to foregoing description method.
Wherein, the mass percent solubility of described copper nano particles is 2-55%.
Wherein, described silver salt is silver nitrate, silver acetate, acetylacetone,2,4-pentanedione silver, silver benzoate, silver citrate, silver cyanate, silver carbonate, silver chlorate, silver propionate, butyric acid silver, valeric acid is silver-colored, caproic acid is silver-colored, enanthic acid is silver-colored, sad silver, enanthic acid silver, actol, silver nitrite, silver thiocyanate, Silver Trifluoroacetate, oleic acid silver-colored or stearic acid silver.
Wherein, described nitrogenous organic ligand is ethylenediamine, 1,2-propane diamine, 1,3-propane diamine, 1,2-butanediamine, 1,3-butanediamine, 1,4-butanediamine, 1,2-heptamethylene diamine, 1,2-hexamethylene diamine, 1,6-hexamethylene diamine, 1,2-cyclohexanediamine, monoethanolamine, Propanolamine, isopropanolamine, 3-aminopropanol, 4-aminobutanol, 2-amino-2-methyl-1-propanol, diglycolamine, diethanol amine, dipropanolamine, pyridine, pyrroles, 2-methvl-pyridinium, 3-methvl-pyridinium or 4-methvl-pyridinium.
Wherein, alcohol organic solvent in described step (1) is methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, n-butanol, ethylene glycol, 1-methyl-ethylene glycol, 1-ethyl-ethylene glycol, 1-butyl-ethylene glycol, 1,3-PD, 1,2-PD, 1,2-butanediol, 1,3-butanediol, BDO, 1,2-pentanediol, 1, any one or multiple mixing of 3-pentanediol, 1,5-PD, 1,6-hexylene glycol or benzylalcohol.
Wherein, organic solvent in described step (2) and step (3) is methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, n-butanol, ethylene glycol, 1-methyl-ethylene glycol, 1-ethyl-ethylene glycol, 1-butyl-ethylene glycol, 1, ammediol, 1,2-propane diols, 1,2-butanediol, 1,3-butanediol, 1,4-butanediol, 1,2-pentanediol, 1, any one or multiple mixing of 3-pentanediol, 1,5-PD, 1,6-hexylene glycol, benzylalcohol, toluene, acetylacetone,2,4-pentanedione, ethyl acetoacetate, oxolane, butanone, cyclopentanone, cyclohexanone.
Solid content is the mass ratio in electrocondution slurry of copper-silver nanometer particle, is not particularly limited.The range of solid content of the copper silver nanoparticle electrocondution slurry that method produced according to the present invention obtains is at 5-75%.
In the present invention, silver complex solution is obtained by silver salt, nitrogenous organic ligand, alcohol organic solvent hybrid reaction.The solubility of silver salt in alcohol organic solvent is less under normal circumstances, and the present invention is by adding organic ligand, greatly can promote the dissolving of silver salt in alcohol organic solvent, thus obtain transparent silver complex solution; Under nitrogen atmosphere, joined again in the dispersion liquid of copper nano particles, silver ion can be made rapidly to evenly spread in the dispersion liquid of copper nano particles, and then there is the reaction of copper reduction silver ion, on deposition of silver to the surface of copper nano particles or be dispersed in reactant liquor, sufficient reacting is allowed to carry out, after question response fully completes, product adopted centrifugal or filter method to be separated, finally product is scattered in organic solvent and obtains copper conductive silver slurry.
" alcohol organic solvent " mentioned in the present invention is the solvent preparing silver complex solution for dissolving silver salt, the alcohol organic solvent that is suitable for comprise methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, n-butanol, ethylene glycol, 1-methyl-ethylene glycol, 1-ethyl-ethylene glycol, 1-butyl-ethylene glycol, 1, ammediol, 1,2-propane diols, 1,2-butanediol, 1,3-butanediol, 1,4-butanediol, 1,2-pentanediol, 1, any one or multiple mixing of 3-pentanediol, 1,5-PD, 1,6-hexylene glycol or benzylalcohol.
" organic solvent " in the present invention in the preparation process of copper nano particles dispersion liquid and copper silver nanoparticle electrocondution slurry as dispersion liquid, the organic solvent that is suitable for comprise methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, n-butanol, ethylene glycol, 1-methyl-ethylene glycol, 1-ethyl-ethylene glycol, 1-butyl-ethylene glycol, 1, ammediol, 1, 2-propane diols, 1, 2-butanediol, 1, 3-butanediol, 1, 4-butanediol, 1, 2-pentanediol, 1, 3-pentanediol, 1, 5-pentanediol, 1, 6-hexylene glycol, benzylalcohol, toluene, acetylacetone,2,4-pentanedione, ethyl acetoacetate, oxolane, butanone, cyclopentanone, any one or multiple mixing of cyclohexanone.The described addition being used as " organic solvent " of dispersion liquid is usual the adopted consumption of those skilled in the art, is not particularly limited in the present invention.
In the present invention, copper nano particles can directly be bought from market or adopt chemical reduction method to synthesize and obtain, as adopted document Nanotechnology 19 (2008) 415604, Journal of Colloid and Interface Science 277 (2004) 100 – 103, the method synthesis reported in Journal of Nanoparticle Research 13 (2011) 127-138, also the method disclosed in Chinese patent (application number 201110355856.7) can be adopted to synthesize obtain, be characterized in that copper nano particles adopts the synthetic method of semi-solid phase heating using microwave to obtain.In the present invention, the synthetic method of copper nano particles is not limited to foregoing description method.
The copper silver nanoparticle electrocondution slurry that the present invention prepares, because copper nano particles is coated by silver, improve the oxidative resistance of electrocondution slurry, and the sintering temperature of electrocondution slurry is low, electrocondution slurry is applicable to the substrates such as polyvinyl chloride (PVC), polyethylene (PE), polyester (PET), nylon (PA), glass, and after sintering, its resistivity is 8.5 × 10
-8-2.5 × 10
-7Ω m, tool has been widely used.
Accompanying drawing explanation
Fig. 1 is the TEM figure of copper galactic nucleus core-shell nanoparticles in the copper silver nanoparticle electrocondution slurry for preparing of the present invention.
specific implementation method
In conjunction with following specific embodiments and the drawings, the present invention is described in further detail, and protection content of the present invention is not limited to following examples.Under the spirit and scope not deviating from inventive concept, the change that those skilled in the art can expect and advantage are all included in the present invention, and are protection domain with appending claims.Implement process of the present invention, condition, reagent, experimental technique etc., except the following content mentioned specially, be universal knowledege and the common practise of this area, be not particularly limited in the present invention.
Embodiment 1
Prepare silver complex solution: be dissolved in by silver salt in the organic solvent of nitrogenous organic ligand and obtain silver complex solution.Concrete steps are: joined by 1.0 grams of silver salt silver nitrates in 6.0 grams of nitrogenous organic ligand ethylenediamines and 8.0 grams of organic solvent n-butanols, at room temperature stir after 30 minutes and obtain silver complex solution.
Embodiment 2-10
Other experiment condition and step are with embodiment 1.Wherein, the kind of silver salt, nitrogenous organic ligand, organic solvent and addition are such as content listed by following table 1.
Embodiment 11
Prepare copper nano particles dispersion liquid: under nitrogen atmosphere, copper nano particles is scattered in organic solvent and obtains copper nano particles dispersion liquid.Concrete steps are: by 25 grams of CuSO
45H
2o is positioned in 800 mL beakers, adds in 20 grams of water, and heating makes CuSO
45H
2o dissolves, and treats CuSO
45H
2after O dissolves completely, add 33.3 grams of PVPs (PVP), after stirring, add 13.2 grams of NaHPO
2xH
2o, after stirring, after placing several minutes at room temperature, obtain the blue semi-solid phase mixture mixed, be positioned in the microwave reaction stove of 700 watts, heating using microwave 30 second, mixture becomes rapidly red copper look, place after 4 minutes, add 50 mL frozen water cancellation reactions, obtained mixture is transferred in centrifuge tube, by copper nano particles centrifugation, the copper nano particles obtained is respectively with 50 mL washing twice, 50 mL ethanol wash twice, finally obtained copper nano particles is dispersed in organic solvent 1-methyl-ethylene glycol, be filled with nitrogen protection, obtain stable copper nano particles dispersion liquid.Wherein, the mass percent solubility of copper nano particles is 2-55%.The addition of above-mentioned organic solvent 1-methyl-ethylene glycol is usual the adopted consumption of those skilled in the art, is not particularly limited in the present embodiment.
Organic solvent can also adopt methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, n-butanol, ethylene glycol, 1-ethyl-ethylene glycol, 1-butyl-ethylene glycol, 1, ammediol, 1,2-propane diols, 1,2-butanediol, 1,3-BDO, 1,4-butanediol, 1,2-pentanediol, 1,3-pentanediol, 1, any one or multiple mixing in 5-pentanediol, 1,6-hexylene glycol, benzylalcohol, toluene, acetylacetone,2,4-pentanedione, ethyl acetoacetate, oxolane, butanone, cyclopentanone, cyclohexanone.Its addition is usual the adopted consumption of those skilled in the art, is not particularly limited.
Embodiment 12
Prepare copper silver nanoparticle electrocondution slurry: at room temperature under an n 2 atmosphere, be added drop-wise in copper nano particles dispersion liquid by silver complex solution and react, reaction product isolated obtains copper silver composite nanometer particle, and is scattered in organic solvent and obtains copper silver nanoparticle electrocondution slurry.Concrete steps are: under nitrogen protection; silver complex solution is added drop-wise in copper nano particles dispersion liquid; at room temperature react after 60 minutes; product is separated by centrifugal method; be dispersed in after washing 2 times with ethanol in organic solvent 1-methyl-ethylene glycol, obtain copper silver nanoparticle electrocondution slurry.The addition of above-mentioned organic solvent 1-methyl-ethylene glycol or other dispersion solvents is usual the adopted consumption of those skilled in the art, is not particularly limited in the present embodiment.
Organic solvent can also adopt methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, n-butanol, ethylene glycol, 1-ethyl-ethylene glycol, 1-butyl-ethylene glycol, 1, ammediol, 1,2-propane diols, 1,2-butanediol, 1,3-BDO, 1,4-butanediol, 1,2-pentanediol, 1,3-pentanediol, 1, any one or multiple mixing in 5-pentanediol, 1,6-hexylene glycol, benzylalcohol, toluene, acetylacetone,2,4-pentanedione, ethyl acetoacetate, oxolane, butanone, cyclopentanone, cyclohexanone.Its addition is usual the adopted consumption of those skilled in the art, is not particularly limited.
In the copper silver nanoparticle electrocondution slurry prepared, on deposition of silver to the surface of copper nano particles or be dispersed in organic solvent reactant liquor, form copper galactic nucleus core-shell nanoparticles as shown in Figure 1.
Embodiment 13-22
The silver complex solution prepared by embodiment 1-10 is added drop-wise in the obtained copper nano particles dispersion liquid of embodiment 11, and prepare copper silver nanoparticle electrocondution slurry according to the method for embodiment 12, its solid content is 5-75%.
The copper silver nanoparticle conductive paste of gained is carried out sintering curing and detected: copper silver nanoparticle electrocondution slurry is coated on sheet glass, sintering curing under nitrogen atmosphere, sintering temperature is 150-250 DEG C, and sintering time is 10 minutes to 60 minutes, obtain conducting film, resistivity is 8.5 × 10
-8-2.5 × 10
-7Ω m, concrete outcome is as shown in table 2 below.
Claims (9)
1. a synthetic method for copper silver nanoparticle electrocondution slurry, is characterized in that, comprises the steps:
(1) silver complex solution is prepared:
Silver salt is dissolved in the alcohol organic solvent of nitrogenous organic ligand and prepares silver complex solution;
(2) copper nano particles dispersion liquid is prepared:
Under nitrogen atmosphere, copper nano particles is scattered in organic solvent obtains copper nano particles dispersion liquid;
(3) copper silver nanoparticle electrocondution slurry is prepared:
At room temperature under an n 2 atmosphere, be added drop-wise in described copper nano particles dispersion liquid by described silver complex solution and react, reaction product isolated obtains copper silver composite nanometer particle, and is scattered in organic solvent and obtains copper silver nanoparticle electrocondution slurry;
Wherein, the molar ratio of described silver salt and nitrogenous organic ligand is 1:1-10.
2. the synthetic method of copper silver nanoparticle electrocondution slurry as claimed in claim 1, it is characterized in that, the mass percent concentration of described silver salt is 4-55%.
3. the synthetic method of copper silver nanoparticle electrocondution slurry as claimed in claim 1, is characterized in that, described copper nano particles adopts the synthetic method of semi-solid phase heating using microwave to prepare.
4. the synthetic method of copper silver nanoparticle electrocondution slurry as claimed in claim 1, it is characterized in that, the mass percent concentration of described copper nano particles is 2-55%.
5. the synthetic method of copper silver nanoparticle electrocondution slurry as claimed in claim 1, it is characterized in that, described silver salt is silver nitrate, silver acetate, acetylacetone,2,4-pentanedione silver, silver benzoate, silver citrate, silver cyanate, silver carbonate, silver chlorate, silver propionate, butyric acid silver, valeric acid is silver-colored, caproic acid is silver-colored, enanthic acid is silver-colored, sad silver, actol, silver nitrite, silver thiocyanate, Silver Trifluoroacetate, oleic acid silver-colored or stearic acid silver.
6. the synthetic method of copper silver nanoparticle electrocondution slurry as claimed in claim 1, it is characterized in that, described nitrogenous organic ligand is ethylenediamine, 1, 2-propane diamine, 1, 3-propane diamine, 1, 2-butanediamine, 1, 3-butanediamine, 1, 4-butanediamine, 1, 2-heptamethylene diamine, 1, 2-hexamethylene diamine, 1, 6-hexamethylene diamine, 1, 2-cyclohexanediamine, monoethanolamine, Propanolamine, isopropanolamine, 3-aminopropanol, 4-aminobutanol, 2-amino-2-methyl-1-propanol, diglycolamine, diethanol amine, dipropanolamine, pyridine, pyrroles, 2-methvl-pyridinium, 3-methvl-pyridinium, or 4-methvl-pyridinium.
7. the synthetic method of copper silver nanoparticle electrocondution slurry as claimed in claim 1, it is characterized in that, alcohol organic solvent in described step (1) is methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, n-butanol, ethylene glycol, 1-methyl-ethylene glycol, 1-ethyl-ethylene glycol, 1-butyl-ethylene glycol, 1, ammediol, 1,2-propane diols, 1,2-butanediol, 1,3-butanediol, 1,4-butanediol, 1,2-pentanediol, 1,3-pentanediol, 1, any one or multiple mixing of 5-pentanediol, 1,6-hexylene glycol or benzylalcohol.
8. the synthetic method of copper silver nanoparticle electrocondution slurry as claimed in claim 1, it is characterized in that, organic solvent in described step (2) and step (3) is methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, n-butanol, ethylene glycol, 1-methyl-ethylene glycol, 1-ethyl-ethylene glycol, 1-butyl-ethylene glycol, 1, ammediol, 1, 2-propane diols, 1, 2-butanediol, 1, 3-butanediol, 1, 4-butanediol, 1, 2-pentanediol, 1, 3-pentanediol, 1, 5-pentanediol, 1, 6-hexylene glycol, benzylalcohol, toluene, acetylacetone,2,4-pentanedione, ethyl acetoacetate, oxolane, butanone, cyclopentanone, any one or multiple mixing in cyclohexanone.
9. the copper silver nanoparticle electrocondution slurry for preparing of method according to claim 1, it is characterized in that, the solid content of described copper silver nanoparticle electrocondution slurry is 5-75%.
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| CN103691965A (en) * | 2013-12-20 | 2014-04-02 | 华南理工大学 | Preparation method for copper/silver heterojunction nano-particles |
| CN104972136B (en) * | 2015-07-30 | 2017-02-01 | 哈尔滨工业大学 | Preparation method for sheet type silver nanoparticles |
| CN105537623B (en) * | 2016-02-01 | 2018-04-17 | 中国科学院深圳先进技术研究院 | A kind of Kufil nanometer sheet and preparation method thereof |
| CN107025950A (en) * | 2016-02-02 | 2017-08-08 | 李文熙 | The preparation method of high conductivity Nano Silver copper-clad inventive thick film paste can be sintered in atmosphere |
| CN114520067B (en) * | 2020-11-20 | 2024-04-05 | 常州明耀半导体科技有限公司 | Conductive paste and transparent display device |
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| US5178909A (en) * | 1990-07-24 | 1993-01-12 | Mitsui Kinzoku Kogyo Kabushiki Kaisha | Production of silver-coated copper-based powders |
| US5945158A (en) * | 1996-01-16 | 1999-08-31 | N.V. Union Miniere S.A. | Process for the production of silver coated particles |
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