CN101569937A - Preparation method for high-dispersing silver powder used for conductive silver paste - Google Patents
Preparation method for high-dispersing silver powder used for conductive silver paste Download PDFInfo
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- CN101569937A CN101569937A CNA2009100746478A CN200910074647A CN101569937A CN 101569937 A CN101569937 A CN 101569937A CN A2009100746478 A CNA2009100746478 A CN A2009100746478A CN 200910074647 A CN200910074647 A CN 200910074647A CN 101569937 A CN101569937 A CN 101569937A
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Abstract
The invention relates to a preparation method for high-dispersing silver powder used for conductive silver paste. Silver nitrate solution and reducer are added into hyper-dispersant solution at the same time under stirring, and the high-dispersing silver powder with different particle diameters from 0.1 to 5.0 mum is obtained by regulating stirring rate and reaction time under the condition of keeping the reaction temperature and pH value of the reaction system unchanged. The method has simple technology; the obtained silver powder has the advantages of high purity, uniform particle diameter, good dispersity and compatibility with macromolecule resin in subsequent procedures, and can be used for preparing conducting coating, conducting paint, conducting resin, and the like.
Description
Technical field
The present invention relates to the preparation method of silver powder, relate in particular to a kind of preparation method who prepares the high dispersive silver powder that conductive silver paste uses.
Background technology
Silver powder itself possesses superior catalytic performance, magnetic property, electrical property etc., thereby in the application that has aspect industry such as aerospace, atomic energy, electronics, powder metallurgy, chemistry and medical science, the bioengineering more and more widely.Silver powder and electric slurry series of products thereof are a kind of noble metal powders that are most widely used in the electronics industry with the consumption maximum, are the fundamental sum key function materials of producing various electronic component products.The electric slurry product integrates metallurgy, chemical industry, electronic technology, it is a kind of electronic functional material of high-tech, be mainly used in and make electromagnetic wave shielding, thick film integrated circuit, resistor, resistor network, capacitor, MLCC, electrically conductive ink, electrode of solar battery, LED cold light source, OLED (OLED), printing and high-resolution electric conductor, thin film switch, flexible circuit, conducting resinl, sensitive components and other electronic devices and components.
The nano-silver powder that is used for the electric slurry industry requires good dispersion, the tap density height, however active high just because of nano-silver powder, the general unresolved agglomeration traits of commercially available so-called nano-silver powder, bad dispersibility very easily take place from sintering or reunion, surface-active is not high, and tap density is low, and organic carrier is difficult to the complete wetting powder during preparation slurry, particle diameter is big, and silver layer is not fine and close behind the sintering, and shrinkage factor is big, and hole is many, poor electrical performance can't satisfy the demand that electronics industry further develops.
The preparation method of silver powder is a lot, can be divided into physics method and chemical method.
The physics method comprises: comminuting method, evaporation-condensation method, atomization etc., there is the shortcomings such as having relatively high expectations, involve great expense to preparation equipment in the physics method.
Chemical method comprises: add thermal decomposition method, gas-phase reaction method, microemulsion method, chemical reduction method etc., chemical method requires lowly to equipment, and easily control is widely used in actual production.
It generally is that liquor argenti nitratis ophthalmicus and reductant solution mixing are carried out reduction reaction that the chemical reduction method of extensive use at present prepares the silver powder process, is settled out silver powder particles.Because silver powder particles is very little, the surface of particle can make and be easy between the particle reunite, so most reduction reaction is to react under the protection of dispersant.But the effect of these dispersants is not fine sometimes, and especially after centrifugation and drying, the reunion of particle is more obvious.
Simultaneously, the silver powder that the existing method that prepare silver powder obtains also exists and the problem for preparing macromolecule resin compatibility difference used in the silver-colored slurry process except that having dispersed bad shortcoming.If when silver powder and mixed with resin, silver powder disperses bad in resin, and then silver slurry performance can not get ensureing.
Chinese patent CN 1785558A number, are called " preparation method of micron grade ball shape silver powder for conductive silver paste " and disclose a technology, and it is that liquor argenti nitratis ophthalmicus is added drop-wise in reducing agent and the dispersant, and regulator solution pH value prepares micron order silver powder simultaneously.The dispersant that this invention is adopted has polyvinylpyrrolidone (PVP), oleic acid, C
8-C
14Aliphatic acid, alkanolamine etc.These traditional dispersants can not guarantee the good dispersion of silver powder particles, and especially after silver powder washing and drying, reunion is more obvious.This can influence the dispersiveness when the preparation electrocondution slurry undoubtedly.
Summary of the invention
Technical problem to be solved by this invention be overcome the defective of prior art and provide a kind of silver powder purity height, particle size evenly, favorable dispersibility and and down-stream in macromolecule resin compatibility favorable conductive silver slurry with the preparation method of high dispersive silver powder.
For solving the problems of the technologies described above, the technical scheme that the present invention takes is:
A kind of preparation method of high-dispersing silver powder used for conductive silver paste, it is under stirring condition, liquor argenti nitratis ophthalmicus and reducing agent are added in the hyper-dispersant solution simultaneously, under the constant situation of the reaction temperature that keeps reaction system and pH value, by adjusting mixing speed and reaction time, obtain the high dispersive silver powder of the different-grain diameter of 0.1～5.0 μ m.
The concentration of described liquor argenti nitratis ophthalmicus is 0.1～2.0mol/l.
Described reducing agent is a kind of or its mixture in ascorbic acid, glucose, formaldehyde, hydrazine hydrate, formic acid or the formates.
The mass ratio of described silver nitrate and hyper-dispersant is 200: 1～5: 1.
Described temperature of reaction system is 10～50 ℃.
Described pH value of reaction system is 2～8.
Described mixing speed is 100～600rpm.
The described reaction time is 1～60 minute.
The present invention adopts reductant solution and liquor argenti nitratis ophthalmicus is joined the method for hyper-dispersant solution simultaneously, rather than adopts general reductant solution is injected in the liquor argenti nitratis ophthalmicus; Perhaps liquor argenti nitratis ophthalmicus is injected in the reductant solution.
According to the colloid chemistry theory, the size of crystal grain and uniformity are mainly by the common decision of the speed of growth of the nucleation rate of crystal and crystal.If reductant solution is injected in the liquor argenti nitratis ophthalmicus; Perhaps liquor argenti nitratis ophthalmicus is injected in the reductant solution, the concentration of silver nitrate or the concentration of reducing agent reduce in course of reaction gradually, and the nucleation rate and the speed of growth are constantly changed, and granular size is inhomogeneous.With the method that reductant solution and liquor argenti nitratis ophthalmicus add simultaneously, help the controllability of reaction speed, make the nucleation rate of particle and the speed of growth reach balance, the size of particle keeps homogeneous.
Characteristics of the present invention also are to use hyper-dispersant (hyperdisperant) rather than traditional dispersant as protective agent, its objective is to avoid silver powder particles to reunite and the compatibility of raising silver powder particles in macromolecule resin.
Hyper-dispersant is a kind of brand-new dispersing aid, and Britain ICI company is adopting this term of hyper-dispersant (hyperdisperant) to describe this kind polymeric dispersant the seventies and eighties in 20th century.To the mid-90, hyper-dispersant is used widely in various fields with its unique function.
Hyper-dispersant and traditional dispersant all have very big difference on structure and dispersion mechanism.The tradition dispersant does not reach the effect that particle disperses with not enough by the absorption affinity on discrete particles surface.And cause particle to flocculate again from the particle surface desorb easily, dispersion stabilization is poor.Simultaneously, the carbochain of traditional dispersant can not produce enough repulsive forces, does not have due stabilization.
Hyper-dispersant is a kind of polymer dispersant that contains anchoring group and solvent chain.Anchoring group includes but are not limited to-R
2,-NR
3 +,-COOH ,-COO
-,-SO
3H ,-SO
3 -,-PO
4 2-, polyamine, polyalcohol and polyethers etc.; Solvent chain includes but are not limited to polyester, polyethers, polyolefin and polyacrylate etc.
In order to reach the good dispersiveness of silver powder particles, the anchoring group of hyper-dispersant must form good adsorption on the silver powder particles surface, and is difficult for desorb in washing process.Just being based on this consideration, the preferred anchoring group of the present invention is-COOH ,-COO
-,-SO
3H ,-SO
3 -,-PO
4 2-, polyamine hyper-dispersant.
In order to make silver powder particles in the silver-colored slurry process of preparation, can good compatibility be arranged with macromolecule resin, according to the similar principle that mixes, select to have the hyper-dispersant of suitable solvent chain according to the different resins selected for use, the mass ratio of silver nitrate and hyper-dispersant is 200: 1～5: 1.
Hyper-dispersant is known by the insider already as a kind of important dispersant, is widely used in industries such as coating, printing ink.There are U.S. Lubrizol company, German BYK company, Denmark KYK company, du pont company etc. in more typical producer, and there are Shanghai three positive scientific ﹠ technical corporation in domestic representative enterprise.
For those oiliness hyper-dispersants, can not dissolve each other with water, so will with surfactant emulsification after use.
Technology of the present invention is simple, the silver powder purity height that obtains, particle size evenly, favorable dispersibility and and down-stream in the macromolecule resin compatibility good.
The specific embodiment
The present invention is described further below in conjunction with specific embodiment.
Embodiment 1
Take by weighing the 15g silver nitrate and be dissolved in the 200ml deionized water, be mixed with liquor argenti nitratis ophthalmicus A; Take by weighing the 18g dissolution of ascorbic acid in the 200ml deionized water, be mixed with reductant solution B; Take by weighing 0.5g Solsperse27000 (production of Lubrizol company) and be dissolved in the 400ml deionized water, be mixed with the hyper-dispersant solution C; C liquid is warmed up to 30 ℃, adjusts speed of agitator to 400rpm; With A liquid and B liquid, be injected in the C liquid, the control injection rate is 25ml/min, continues to stir 20min after injection is finished, keeping temperature simultaneously is 30 ℃.Use centrifuge with Separation of Solid and Liquid.Deionized water and acetone wash respectively 3 times, after the Separation of Solid and Liquid, silver powder are carried out vacuum drying at 60 ℃, obtain 1
#Silver powder.
Embodiment 2
Take by weighing the 16g silver nitrate and be dissolved in the 150ml deionized water, be mixed with liquor argenti nitratis ophthalmicus A; Take by weighing the 30g ammonium formate and be dissolved in the 150ml deionized water, be mixed with reductant solution B; Take by weighing 0.9g Solsperse20000 (production of Lubrizol company) and be dissolved in the 400ml deionized water, be mixed with the hyper-dispersant solution C; C liquid is warmed up to 40 ℃, adjusts speed of agitator to 300rpm; A liquid and B liquid at the uniform velocity are injected into C liquid, and remain unchanged always; The adjustment injection rate is 30ml/min; After finishing, injection continues to keep 30min; Use centrifuge with Separation of Solid and Liquid.Use deionized water and acetone to wash respectively 3 times, after the Separation of Solid and Liquid, silver powder is carried out vacuum drying at 60 ℃, obtain 2
#Silver powder.
Embodiment 3
Take by weighing the 10g silver nitrate and be dissolved in the 150ml deionized water, be mixed with liquor argenti nitratis ophthalmicus A; Take by weighing the 13g dissolution of ascorbic acid in the 150ml deionized water, be mixed with reductant solution B; Take by weighing 0.8g CH-10 (Shanghai three positive macromolecular material companies produce) and be dissolved in the 350ml deionized water, be mixed with the hyper-dispersant solution C; It is 300rpm that C liquid is adjusted speed of agitator; Be warmed up to 25 ℃ simultaneously, and remain unchanged always; A liquid and B liquid are injected in the C mixed liquor simultaneously, and the adjustment injection rate is 30ml/min; After finishing, injection continues to keep 30min; Use centrifuge with Separation of Solid and Liquid.Use deionized water and acetone to wash respectively 3 times, after the Separation of Solid and Liquid, silver powder is carried out vacuum drying at 60 ℃, obtain 3
#Silver powder.
Embodiment 4
Take by weighing the 15g silver nitrate and be dissolved in the 150ml deionized water, be mixed with liquor argenti nitratis ophthalmicus A; Take by weighing the 20g dissolution of ascorbic acid in the 150ml deionized water, be mixed with reductant solution B; Take by weighing 0.4g CH-13 (Shanghai three positive macromolecular material companies produce) and peregal os-15 0.1g and be dissolved in the 400ml deionized water, be mixed with the hyper-dispersant solution C after fully stirring; It is 200rpm that C liquid is adjusted speed of agitator; Be warmed up to 25 ℃ simultaneously, and remain unchanged always; A liquid and B liquid are injected in the C mixed liquor simultaneously, and the adjustment injection rate is 25ml/min; After finishing, injection continues to keep 30min; Use centrifuge with Separation of Solid and Liquid.Use deionized water and acetone to wash respectively 3 times, after the Separation of Solid and Liquid, silver powder is carried out vacuum drying at 60 ℃, obtain 4
#Silver powder.
Embodiment 5
Take by weighing the 15g silver nitrate and be dissolved in the 250ml deionized water, be mixed with liquor argenti nitratis ophthalmicus A; Take by weighing the 20g hydrazine hydrate and be dissolved in the 250ml deionized water, be mixed with reductant solution B; Take by weighing 2.0g CH-1 (Shanghai three positive macromolecular material companies produce) and peregal OS-20 0.4g and be dissolved in the 300ml deionized water, be mixed with the hyper-dispersant solution C after fully stirring; It is 200rpm that C liquid is adjusted speed of agitator; Be warmed up to 25 ℃ simultaneously, and remain unchanged always; A liquid and B liquid are injected in the C mixed liquor simultaneously, and the adjustment injection rate is 25ml/min; After finishing, injection continues to keep 30min; Use centrifuge with Separation of Solid and Liquid.Use deionized water and acetone to wash respectively 3 times, after the Separation of Solid and Liquid, silver powder is carried out vacuum drying at 60 ℃, obtain 5
#Silver powder.
Comparative Examples
Take by weighing the 15g silver nitrate and 1.2g PVP (polyvinylpyrrolidone) is dissolved in the 200ml deionized water, be mixed with liquor argenti nitratis ophthalmicus A; Take by weighing the 20g hydrazine hydrate and be dissolved in the 200ml deionized water, be mixed with reductant solution B; It is 200rpm that B liquid is adjusted speed of agitator; Be warmed up to 30 ℃ simultaneously, and remain unchanged always; A liquid is injected in the B liquid, and the adjustment injection rate is 25ml/min; After finishing, injection continues to keep 30min; Use centrifuge with Separation of Solid and Liquid.Use deionized water and acetone to wash respectively 3 times, after the Separation of Solid and Liquid, silver powder is carried out vacuum drying at 60 ℃, obtain Comparative Examples silver powder.
According to GB GB/T 1773-1995 appendix A " the emission spectrographic analysis method of impurity element in the fine silver " silver powder is carried out dirt content test; Above-mentioned silver powder is carried out TEM (transmission electron microscope) and SEM (ESEM) analysis, obtain particle diameter, shape, the dispersed index of silver powder; The results are shown in following table:
| Embodiment | Grain shape | Purity | Particle size range | Dispersed | Compatibility |
| Embodiment 1 | Spherical | 99.97％ | 0.2-0.5 | Well | Well |
| Embodiment 2 | Spherical | 99.97％ | 0.3-0.6 | Well | Well |
| Embodiment 3 | Spherical | 99.97％ | 1.2-3.5 | Well | Well |
| Embodiment 4 | The class sphere | 99.97％ | 2.0-5.0 | Well | Well |
| Embodiment 5 | The class sphere | 99.97％ | 1.0-2.5 | Well | Well |
| Comparative Examples | The class sphere | 99.95％ | 0.5-2.5 | Difference | Difference |
By the data in the table as can be seen, the purity height, particle size of taking the silver powder of method provided by the invention preparation evenly, favorable dispersibility and and down-stream in the macromolecule resin compatibility good.
Claims (8)
1. the preparation method of a high-dispersing silver powder used for conductive silver paste, it is characterized in that: it is under stirring condition, liquor argenti nitratis ophthalmicus and reducing agent are added in the hyper-dispersant solution simultaneously, under the constant situation of the reaction temperature that keeps reaction system and pH value, by adjusting mixing speed and reaction time, obtain the high dispersive silver powder of the different-grain diameter of 0.1～5.0 μ m.
2. according to the preparation method of the described high-dispersing silver powder used for conductive silver paste of claim 1, it is characterized in that: the concentration of described liquor argenti nitratis ophthalmicus is 0.1～2.0mol/l.
3. according to the preparation method of the described high-dispersing silver powder used for conductive silver paste of claim 2, it is characterized in that: described reducing agent is a kind of or its mixture in ascorbic acid, glucose, formaldehyde, hydrazine hydrate, formic acid or the formates.
4. according to the preparation method of the described high-dispersing silver powder used for conductive silver paste of claim 3, it is characterized in that: the mass ratio of described silver nitrate and hyper-dispersant is 200: 1～5: 1.
5. according to the preparation method of the described high-dispersing silver powder used for conductive silver paste of claim 4, it is characterized in that: described temperature of reaction system is 10～50 ℃.
6. according to the preparation method of the described high-dispersing silver powder used for conductive silver paste of claim 5, it is characterized in that: described pH value of reaction system is 2～8.
7. according to the preparation method of the described high-dispersing silver powder used for conductive silver paste of claim 6, it is characterized in that: described mixing speed is 100～600rpm.
8. according to the preparation method of the described high-dispersing silver powder used for conductive silver paste of claim 7, it is characterized in that: the described reaction time is 1～60 minute.
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