CN103551586B - A kind of preparation method of micron spherical silver powder for electroconductive silver paste - Google Patents
A kind of preparation method of micron spherical silver powder for electroconductive silver paste Download PDFInfo
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- CN103551586B CN103551586B CN201310429617.0A CN201310429617A CN103551586B CN 103551586 B CN103551586 B CN 103551586B CN 201310429617 A CN201310429617 A CN 201310429617A CN 103551586 B CN103551586 B CN 103551586B
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Abstract
The present invention relates to a kind of preparation method of micron spherical silver powder for electroconductive silver paste, the method controls liquor argenti nitratis ophthalmicus and has identical pH value and temperature with reductant solution, therefore, no matter be adopt a kind of mode joining another kind of solution in liquor argenti nitratis ophthalmicus and reductant solution, or adopt the mode that two kinds of solution drips simultaneously, the pH value of system and temperature all can not change, and pH value and temperature are as affecting the maximum factor of particle diameter, make the silver powder obtained have more uniform particle diameter.And based on same reason, after two kinds of solution all join reactor, only need of short duration mixing time can complete the reaction generating silver powder, therefore this method production efficiency is high.The micron spherical silver powder particle diameter obtained by this method is between 0.1 ~ 5 μm, and the apparent density of silver powder is not less than 2.80g/cm
3, tap density is not less than 5.0g/cm
3; Be suitable as the electric conductor in silver paste of solar cells and other high temperature sintering types silver slurry.
Description
Technical field
The present invention relates to the preparation method of silver powder, be specifically related to a kind of preparation method of micron spherical silver powder for electroconductive silver paste.
Background technology
Electric slurry product, as a kind of electronic functional material, is mainly used to manufacture electromagnetic wave shielding, electrode of solar battery, flexible circuit and other electronic devices and components.Electric slurry requires higher to every physics of conductive silver paste, chemical property, and being therefore prepared in whole operation of electrocondution slurry metal dust seems particularly important.The preparation method of super fine silver powder has a variety of, and wherein chemical reduction method is the most general method being used for preparing micron-grade superfine silver powder.The key problem in technology producing super fine silver powder how to control its particle size, size distribution and pattern when producing in batches.
Publication number preparation method disclosed in the Chinese patent of CN 1387968 is difficult to the pH value of the hierarchy of control, be not suitable for for large-scale industrial production, and reducing agent mixed solution is poured into liquor argenti nitratis ophthalmicus mixing and is reacted by this invention, should not the nucleation of control Ag grain and the growth of nucleus.Application number preparation method disclosed in the Chinese patent of 200510095739.6 adopts and is added drop-wise in reduction system by liquor argenti nitratis ophthalmicus, about making whole reduction process be stabilized in a pH value by the rate of addition of adjustment ammoniacal liquor simultaneously; But because the pH value of liquor argenti nitratis ophthalmicus is not identical with the pH value of reduction system, in order to avoid pH value change is too fast, need the rate of addition controlling liquor argenti nitratis ophthalmicus, and need 25 ~ 30 minutes just can complete reaction after being added dropwise to complete, production efficiency is low.The preparation method of application number high-dispersing silver powder used for conductive silver paste disclosed in the Chinese patent of 200910074647.8 adopts and adds in hyper-dispersant solution by reductant solution and liquor argenti nitratis ophthalmicus simultaneously, this method is conducive to the controlled of reaction speed, make the nucleation rate of particle and the speed of growth reach balance, obtain the size of silver powder particles 0.2 ~ 1
μm.But for the preparation of silver slurry used for solar batteries, the tap density of this glass dust is low, and particle diameter is too small, cause the conductance of silver slurry not high enough, the solar battery efficiency being starched preparation by this silver is low, is no more than 15.2%.
Summary of the invention
The technical issues that need to address of the present invention are the preparation method providing a kind of micron spherical silver powder for electroconductive silver paste, and this method production efficiency is high, and the conductive silver powder obtained is subsphaeroidal, and domain size distribution is 0.1 ~ 5.0
μin the scope of m.
The technical issues that need to address of the present invention are achieved through the following technical solutions:
A preparation method for micron spherical silver powder for electroconductive silver paste, the method comprises the following steps successively:
(1) reductant solution and liquor argenti nitratis ophthalmicus nitric acid and/or ammoniacal liquor are adjusted to identical pH value and temperature, wherein pH value is 3 ~ 6, and temperature is 30 ~ 60 DEG C, has at least a kind of solution to be added with dispersant in reductant solution and liquor argenti nitratis ophthalmicus;
(2) by liquor argenti nitratis ophthalmicus and reductant solution while stirring liquid feeding mix, and keep mixeding liquid temperature to be 30 ~ 60 DEG C;
(3) liquid feeding complete after continuation stirring 1 ~ 20 minute, form silver powder suspension;
(4) silver powder suspension is filtered, the silver powder after filtering is carried out washing and drying;
(5) silver powder after drying is crossed 300 ~ 500 mesh sieves and obtain 0.1 ~ 5.0
μm conductive submicron ball shape silver powder.
As the technical scheme of a modification of the present invention, when liquor argenti nitratis ophthalmicus being mixed with reductant solution in described step (2), liquor argenti nitratis ophthalmicus and reductant solution are respectively joined in reactor with the liquid feeding speed of 50 ~ 150ml/ second simultaneously.
As the technical scheme that another kind of the present invention improves, when liquor argenti nitratis ophthalmicus being mixed with reductant solution in described step (2), first liquor argenti nitratis ophthalmicus is added in reactor, then in reactor, add reductant solution with the liquid feeding speed of 50 ~ 150ml/ second.
In above-mentioned three kinds of basic technical schemes, preferably, in described step (1), the concentration of liquor argenti nitratis ophthalmicus is 80 ~ 150g/L, and the concentration of reductant solution is 50 ~ 250g/L.
Further preferably, in described step (1), reducing agent is the one in hydrazine hydrate, glucose, formaldehyde and ascorbic acid, and dispersant is the one in PVP, PVA, gelatin and oleic acid.
In above-mentioned three kinds of basic technical schemes, preferably, the time that in described step (3), liquid feeding continues to stir after completing is 1 ~ 5 minute.
In above-mentioned three kinds of basic technical schemes, preferably, washing process is in described step (4): with deionized water wash 2 ~ 4 times, absolute ethyl alcohol washes 2 ~ 4 times, total washing water consumption is 500 ± 100ml/10g Ag, and total alcohol wash consumption is 160 ± 40ml/10g Ag.
In above-mentioned three kinds of basic technical schemes, preferably, in described step (4), drying condition is: forced air drying 6 ~ 12 hours at 60 ± 3 DEG C.
Compared with prior art, advantage of the present invention and beneficial effect are:
1, the preparation method of micron spherical silver powder for electroconductive silver paste of the present invention, the method controls liquor argenti nitratis ophthalmicus and has identical pH value and temperature with reductant solution, therefore, no matter be adopt a kind of mode joining another kind of solution in liquor argenti nitratis ophthalmicus and reductant solution, or adopt the mode that two kinds of solution drips simultaneously, the pH value of system and temperature all can not change, and pH value and temperature are as affecting the maximum factor of particle diameter, make the silver powder obtained have more uniform particle diameter.The micron spherical silver powder particle diameter obtained by this method is 0.1 ~ 5
μbetween m.
2, the preparation method of micron spherical silver powder for electroconductive silver paste of the present invention, because the pH value of solution system in liquor argenti nitratis ophthalmicus in the method and reductant solution mixed process and temperature do not change, therefore after two kinds of solution all join reactor, only need of short duration mixing time can complete the reaction generating silver powder, thus shorten the production time of silver powder, improve life efficiency.Compared with prior art, after two kinds of solution all join reactor, only need less than 20 minutes, even only need can complete less than 5 minutes the reaction generating silver powder under preferred reaction condition.
3, the preparation method of micron spherical silver powder for electroconductive silver paste of the present invention, because the method adopts conventional dispersant, the silver powder particle diameter obtained is 0.1 ~ 5
μbetween m, the apparent density of silver powder is not less than 2.80g/cm
3, tap density is not less than 5.0 g/cm
3; Be suitable as very much the electric conductor in silver paste of solar cells and other high temperature sintering types silver slurry.
Detailed description of the invention
Below in conjunction with embodiment, the specific embodiment of the present invention is described further.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
The present invention is a kind of preparation method of micron spherical silver powder for electroconductive silver paste, and the method is a kind of chemical reduction method.
The feature of the preparation method of micron spherical silver powder for electroconductive silver paste of the present invention is: control liquor argenti nitratis ophthalmicus and have identical pH value and temperature with reductant solution, therefore, no matter be adopt a kind of mode joining another kind of solution in liquor argenti nitratis ophthalmicus and reductant solution, or adopt the mode that two kinds of solution drips simultaneously, the pH value of system and temperature all can not change, and pH value and temperature are as affecting the maximum factor of particle diameter, the silver powder obtained is made to have more uniform particle diameter.In addition, because the pH value of solution system in liquor argenti nitratis ophthalmicus in the method and reductant solution mixed process and temperature do not change, therefore after two kinds of solution all join reactor, only need of short duration mixing time can complete the reaction generating silver powder, thus shorten the production time of silver powder, improve production efficiency.
Embodiment 1
The present invention is a kind of preparation method of micron spherical silver powder for electroconductive silver paste, and it comprises the following steps successively:
(1) prepare the liquor argenti nitratis ophthalmicus of 100g/L, dripping nitric acid adjust ph is 3, is incubated at 50 DEG C; Reducing agent is ascorbic acid, and the reductant solution of preparation 80g/L, is 3 by nitric acid and ammoniacal liquor adjust ph, is incubated at 50 DEG C; The reductant solution getting the liquor argenti nitratis ophthalmicus of 500ml and 500ml is stand-by; Get 5g PVP as dispersant, join in liquor argenti nitratis ophthalmicus.
(2) liquor argenti nitratis ophthalmicus and reductant solution joined with the liquid feeding speed of 100ml/ second and be furnished with in the reactor of agitator, stir liquid feeding mixing, mixing speed is 100 revs/min, and keeps mixeding liquid temperature to be 50 DEG C.
(3) liquid feeding complete after continuation stirring 3 minutes, form silver powder suspension.
(4) silver powder suspension is filtered, silver powder deionized water after filtering is washed 3 times, absolute ethyl alcohol washes 3 times, total washing water consumption is 500 ± 100ml/10g Ag, and total alcohol wash consumption is 160 ± 40ml/10g Ag, then forced air drying 9 hours at 60 ± 3 DEG C.
(5) silver powder after drying is crossed 300 ~ 500 mesh sieves and obtain 0.1 ~ 5.0
μm conductive submicron ball shape silver powder.
Embodiment 2
The present invention is a kind of preparation method of micron spherical silver powder for electroconductive silver paste, and it comprises the following steps successively:
(1) prepare the liquor argenti nitratis ophthalmicus of 150g/L, dripping nitric acid adjust ph is 6, is incubated at 30 DEG C; Reducing agent is glucose, and the reductant solution of preparation 250g/L, is 6 by nitric acid and ammoniacal liquor adjust ph, is incubated at 30 DEG C; The reductant solution getting the liquor argenti nitratis ophthalmicus of 500ml and 500ml is stand-by; Get 8g PVA as dispersant, join in reductant solution.
(2) liquor argenti nitratis ophthalmicus is all added be furnished with in the reactor of agitator, again reductant solution is added in reactor with the liquid feeding speed of 150ml/ second, stir while liquid feeding mixing, mixing speed is 100 revs/min, and keeps mixeding liquid temperature to be 30 DEG C;
(3) liquid feeding complete after continuation stirring 20 minutes, form silver powder suspension;
(4) silver powder suspension is filtered, silver powder deionized water after filtering is washed 4 times, absolute ethyl alcohol washes 2 times, total washing water consumption is 500 ± 100ml/10g Ag, and total alcohol wash consumption is 160 ± 40ml/10g Ag, then forced air drying 12 hours at 60 ± 3 DEG C;
(5) silver powder after drying is crossed 300 ~ 500 mesh sieves and obtain 0.1 ~ 5.0
μm conductive submicron ball shape silver powder.
Embodiment 3
The present invention is a kind of preparation method of micron spherical silver powder for electroconductive silver paste, and it comprises the following steps successively:
(1) prepare the liquor argenti nitratis ophthalmicus of 80g/L, dripping nitric acid adjust ph is 4, is incubated at 60 DEG C; Reducing agent is hydrazine hydrate, and the reductant solution of preparation 50g/L, is 4 by nitric acid and ammoniacal liquor adjust ph, is incubated at 60 DEG C; The reductant solution getting the liquor argenti nitratis ophthalmicus of 500ml and 500ml is stand-by; Get 4g oleic acid as dispersant, join in liquor argenti nitratis ophthalmicus.
(2) liquor argenti nitratis ophthalmicus is all added be furnished with in the reactor of agitator, then reductant solution is added in reactor with the liquid feeding speed of 50ml/ second, stir liquid feeding mixing, and keep mixeding liquid temperature to be 60 DEG C;
(3) liquid feeding complete after continuation stirring 1 minute, form silver powder suspension;
(4) silver powder suspension is filtered, silver powder deionized water after filtering is washed 2 times, absolute ethyl alcohol washes 4 times, total washing water consumption is 500 ± 100ml/10g Ag, and total alcohol wash consumption is 160 ± 40ml/10g Ag, then forced air drying 6 hours at 60 ± 3 DEG C;
(5) silver powder after drying is crossed 300 ~ 500 mesh sieves and obtain 0.1 ~ 5.0
μm conductive submicron ball shape silver powder.
Embodiment 4
The present invention is a kind of preparation method of micron spherical silver powder for electroconductive silver paste, and it comprises the following steps successively:
(1) prepare the liquor argenti nitratis ophthalmicus of 120g/L, dripping nitric acid adjust ph is 5, is incubated at 40 DEG C; Reducing agent is formaldehyde, and the reductant solution of preparation 100g/L, is 5 by nitric acid and ammoniacal liquor adjust ph, is incubated at 40 DEG C; The reductant solution getting the liquor argenti nitratis ophthalmicus of 500ml and 500ml is stand-by; Get 4.5g gelatin as dispersant, join in liquor argenti nitratis ophthalmicus.
(2) liquor argenti nitratis ophthalmicus and reductant solution joined with the liquid feeding speed of 120ml/ second and be furnished with in the reactor of agitator, stir liquid feeding mixing, mixing speed is 100 revs/min, and keeps mixeding liquid temperature to be 40 DEG C.
(3) liquid feeding complete after continuation stirring 5 minutes, form silver powder suspension;
(4) silver powder suspension is filtered, silver powder deionized water after filtering is washed 3 times, absolute ethyl alcohol washes 2 times, total washing water consumption is 500 ± 100ml/10g Ag, and total alcohol wash consumption is 160 ± 40ml/10g Ag, then forced air drying 7 hours at 60 ± 3 DEG C;
(5) silver powder after drying is crossed 300 ~ 500 mesh sieves and obtain 0.1 ~ 5.0
μm conductive submicron ball shape silver powder.
The particle size range of embodiment 1 ~ 4 gained silver powder, apparent density and tap density test result are listed in table 1.And by the silver powder that obtains in embodiment 1 ~ 4 and terpinol, ethyl cellulose and glass dust according to the weight ratio of 75:10:5:5 after three-roller mixes, be printed on monocrystalline silicon piece, be assembled into battery according to the technique of solar cell, analyzer electricity conversion, result also lists in table 1.From table 1, the particle diameter of gained silver powder is all 0.1 ~ 5
μbetween m, apparent density is not less than 2.80g/cm
3, tap density is not less than 5.0 g/cm
3, electricity conversion is close to A level level (18%).
Table 1:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Grain shape | Spherical | Spherical | Spherical | Spherical |
| Purity | 99.97% | 99.97% | 99.97% | 99.97% |
| Particle size range ( μm) | 0.2~4.6 | 0.1~5 | 0.3~4.3 | 0.2~4.7 |
| Apparent density (g/cm 3) | 2.93 | 2.82 | 2.84 | 2.97 |
| Tap density (g/cm 3) | 5.16 | 5.06 | 5.07 | 5.12 |
| Electricity conversion (%) | 17.8 | 17.9 | 17.5 | 17.7 |
Above-mentioned each embodiment is further illustrating of making foregoing of the present invention, but the scope that should not be construed as the above-mentioned theme of the present invention is only limitted to above-described embodiment.It should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. a preparation method for micron spherical silver powder for electroconductive silver paste, is characterized in that: the method comprises the following steps successively:
(1) reductant solution and liquor argenti nitratis ophthalmicus nitric acid and/or ammoniacal liquor are adjusted to identical pH value and temperature, wherein pH value is 3 ~ 6, and temperature is 30 ~ 60 DEG C, has at least a kind of solution to be added with dispersant in reductant solution and liquor argenti nitratis ophthalmicus;
(2) by liquor argenti nitratis ophthalmicus and reductant solution while stirring liquid feeding mix, and keep mixeding liquid temperature to be 30 ~ 60 DEG C;
(3) liquid feeding complete after continuation stirring 1 ~ 20 minute, form silver powder suspension;
(4) silver powder suspension is filtered, the silver powder after filtering is carried out washing and drying;
(5) silver powder after drying is crossed 300 ~ 500 mesh sieves and obtain 0.1 ~ 5.0
μm conductive submicron ball shape silver powder.
2. preparation method as claimed in claim 1, it is characterized in that: when liquor argenti nitratis ophthalmicus being mixed with reductant solution in described step (2), liquor argenti nitratis ophthalmicus and reductant solution are respectively joined in reactor with the liquid feeding speed of 50 ~ 150ml/ second simultaneously.
3. preparation method as claimed in claim 1, it is characterized in that: when liquor argenti nitratis ophthalmicus being mixed with reductant solution in described step (2), first liquor argenti nitratis ophthalmicus is added in reactor, then in reactor, add reductant solution with the liquid feeding speed of 50 ~ 150ml/ second.
4. the preparation method as described in claims 1 to 3 any one, is characterized in that: in described step (1), the concentration of liquor argenti nitratis ophthalmicus is 80 ~ 150g/L, and the concentration of reductant solution is 50 ~ 250g/L.
5. preparation method as claimed in claim 4, is characterized in that: in described step (1), reducing agent is the one in hydrazine hydrate, glucose, formaldehyde and ascorbic acid, and dispersant is the one in PVP, PVA, gelatin and oleic acid.
6. the preparation method as described in claims 1 to 3 any one, is characterized in that: the time that in described step (3), liquid feeding continues to stir after completing is 1 ~ 5 minute.
7. the preparation method as described in claims 1 to 3 any one, it is characterized in that: washing process is in described step (4): with deionized water wash 2 ~ 4 times, absolute ethyl alcohol washes 2 ~ 4 times, total washing water consumption is 500 ± 100ml/10g Ag, and total alcohol wash consumption is 160 ± 40ml/10g Ag.
8. the preparation method as described in claims 1 to 3 any one, is characterized in that: in described step (4), drying condition is: forced air drying 6 ~ 12 hours at 60 ± 3 DEG C.
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| CN103079726A (en) * | 2010-08-30 | 2013-05-01 | E·I·内穆尔杜邦公司 | Silver particles and a process for making them |
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