CN105345027B - A kind of high-dispersion submicron silver powder production method - Google Patents
A kind of high-dispersion submicron silver powder production method Download PDFInfo
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- CN105345027B CN105345027B CN201510851075.5A CN201510851075A CN105345027B CN 105345027 B CN105345027 B CN 105345027B CN 201510851075 A CN201510851075 A CN 201510851075A CN 105345027 B CN105345027 B CN 105345027B
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Abstract
The invention discloses a kind of high-dispersion submicron silver powder production method, comprise the following steps：1）Prepare colloidal solution A；2）Sodium ascorbate, dissolving are added in colloidal solution A；3）Again plus hydrogenperoxide steam generator, reductant solution is obtained；4）Prepare colloidal solution B；5）Plus silver nitrate, obtain being reduced solution；6）Solution will be reduced to be added in reductant solution, produced after the completion of reaction.The present invention, as reducing agent, produces the evengranular silver powder for being less than 0.5 micron using sodium ascorbate；Hydration status by the use of natural peach gum are used as dispersion, it is ensured that the dispersity of product；Using hydrogen peroxide is added in reaction system, i.e., using its reproducibility, its corrosivity is utilized again, on the premise of or else destroying original reduction system, the organic coating thing content of product is reduced, so as to improve electrical property of the product in slurry system.
Description
Technical field
The present invention relates to electric slurry field, a kind of high-dispersion submicron silver powder production method is specifically referred to.
Background technology
With the prevalence of electronics wearable device, the requirement more and more higher to electronic equipment microminiaturization, accordingly to printing electricity
The requirement of sub-line road and printing electronic circuit is more and more thinner, and line spacing is less and less, therefore silver powder particles are also required that increasingly
Small, the demand that in the market is less than 1 micron of silver powder particles to particle diameter is in steady increasing trend, has greatly promoted production sub-micron
The development of the silver powder technology of particle.
Also there is more deficiency in the silver powder technology of existing production submicron particles, the particle diameter of the silver powder particles produced first
Between 0.6 ~ 1 micron, the application demand of electronic product can not be also met；Secondly, it is micro- less than 0.5 even if producing particle diameter
The silver powder particles of rice, but because the particle of submicron silver powder is too small, specific surface area is excessive, so there is very serious reunion in silver powder
Situation, it is impossible to disperse well in slurry system；Finally, good dispersion, particle are synthesized using macromolecular hydrated colloidal
Desired silver powder product is met, but due to the presence of a large amount of organic coating things, has had a strong impact on the electric conductivity of silver powder particles, from
And the performance of terminal slurry products is have impact on, it is not applied well.
The content of the invention
It is an object of the invention to provide a kind of submicron silver powder that can obtain uniform particle sizes, while silver powder can also be reduced
Surface organic matter coating content, improves electric conductivity, reduces the high-dispersion submicron silver powder production method of content of organics.
The present invention is achieved through the following technical solutions：A kind of high-dispersion submicron silver powder production method, it is characterised in that bag
Include following steps：
（1）The natural peach gums of 8.5 ~ 12.5kg are added in 200 ~ 350L deionized waters, disperses 1 ~ 2h, prepares colloidal solution A；
（2）Sodium ascorbate is added into colloidal solution A, is stirred continuously to being completely dissolved；
（3）Hydrogenperoxide steam generator is added, reductant solution is obtained after being uniformly mixed；
（4）The natural peach gums of 1.2 ~ 2.5kg are added in 30 ~ 60L deionized waters, disperses 1 ~ 2h, prepares colloidal solution B；
（5）Silver nitrate is added in colloidal solution B, obtains being reduced solution after stirring to its all dissolving；
（6）Solution will be reduced to be added in reductant solution, produced after the completion of reaction.
The technical program is by the use of sodium ascorbate as reducing agent, using natural peach gum as dispersant, and synthesis 0.1-0.4 is micro-
The evengranular silver powder particles of rice.While synthetic reaction, another reducing agent hydrogen peroxide is added, its corrosion is utilized
Property gets rid of the organic matter on silver powder surface, evengranular submicron silver powder is obtained so as to generate, while its table can also be reduced
Face Coated with Organic Matter thing content, so that high conductivity is obtained, the high-dispersion submicron silver powder product of low content of organics.
Method in order to which the present invention is better achieved, further, comprises the following steps：
（1）The natural peach gums of 8.5 ~ 12.5kg are added in 200 ~ 350L deionized waters, disperses 1 ~ 2h, prepares colloidal solution A；
（2）Colloidal solution A temperature is adjusted to 45 ~ 60 DEG C, 15 ~ 25kg sodium ascorbates are then added thereto, are constantly stirred
Mix to being completely dissolved；
（3）Again to being dissolved with the colloidal solution A of sodium ascorbate, the peroxide that 5.0 ~ 9.5L mass fractions are 20% is added
Change hydrogen solution, reductant solution is obtained after being uniformly mixed；
（4）The natural peach gums of 1.2 ~ 2.5kg are added in 30 ~ 60L deionized waters, disperses 1 ~ 2h, prepares colloidal solution B；
（5）15 ~ 25kg silver nitrates are added in colloidal solution B, obtain being reduced solution after stirring to its all dissolving；
（6）Solution will be reduced to be added in reductant solution with 0.2 ~ 0.3L/min speed, produced after the completion of reaction.
Method in order to which the present invention is better achieved, further, the step（1）In, prepare the specific of colloidal solution A
Process is that the specific consumption of natural peach gum is 10.0kg, and the specific consumption of deionized water is 200L, and jitter time is 1h.
Method in order to which the present invention is better achieved, further, the step（2）In, detailed process is, colloid is molten
Liquid A temperature is adjusted to 50 ~ 55 DEG C, 20.0kg sodium ascorbates is then added thereto, and be stirred continuously to being completely dissolved.
Method in order to which the present invention is better achieved, further, the step（3）In, the hydrogenperoxide steam generator of addition
Mass fraction be 20%, and add hydrogenperoxide steam generator amount be 7.5L.
Method in order to which the present invention is better achieved, further, the step（1）, step（2）, step（3）Process
It is to be carried out in 500L reactor.
Method in order to which the present invention is better achieved, further, the step（4）In, prepare the specific of colloidal solution B
Process is that the specific consumption of natural peach gum is 1.5kg, and the specific consumption of deionized water is 53L, and jitter time is 1h.
Method in order to which the present invention is better achieved, further, the step（5）In, it is necessary to add silver nitrate be
20kg。
Method in order to which the present invention is better achieved, further, the step（4）And step（5）Process be
Carried out in 100L reactor.
Method in order to which the present invention is better achieved, further, the step（6）In, will be reduced solution with
0.25L/min speed is added in reductant solution.
The present invention compared with prior art, with advantages below and beneficial effect：
（1）The present invention, as reducing agent, produces the evengranular silver powder for being less than 0.5 micron using sodium ascorbate；
（2）The present invention is used as dispersion by the use of the hydration status of natural peach gum, it is ensured that the dispersity of product.
（3）The present invention in reaction system using hydrogen peroxide is added, i.e., using its reproducibility, and its corrosivity is utilized again, then
On the premise of not destroying original reduction system, the organic coating thing content of product is reduced, so as to improve product in slurry system
In electrical property.
Brief description of the drawings
By reading the detailed description made with reference to the following drawings to non-limiting example, other features of the invention,
Objects and advantages will be changed to substantially：
Fig. 1 is the scanning electron microscope (SEM) photograph of inventive method products obtained therefrom；
Fig. 2 is the scanning electron microscope (SEM) photograph that inventive method products obtained therefrom further amplifies.
Embodiment
The present invention is described in further detail with reference to embodiment, but the implementation of the present invention is not limited to this,
Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and customary means, various replace is made
Change and change, all should be included within the scope of the invention.
Embodiment 1：
The present embodiment, prepares two kinds of colloidal solution, and by sodium ascorbate and be added thereto a kind of glue using natural peach gum
In liquid solution, hydrogenperoxide steam generator is being added, reductant solution is obtained；Silver nitrate is added into another colloidal solution again, is made
It is reduced solution；Finally, solution will be reduced to add in reductant solution, reacted, and the peroxidating added in reducing agent
Hydrogen has corrosivity, can remove the organic matter on silver powder surface, and evengranular submicron silver powder is obtained so as to generate, also simultaneously
Its surface organic matter coating content can be reduced, so that high conductivity is obtained, the high-dispersion submicron silver of low content of organics
Powder product.
Specific implementation step is：
（1）The natural peach gums of 8.5 ~ 12.5kg are added in 200 ~ 350L deionized waters, disperses 1 ~ 2h, prepares colloidal solution A；
（2）Sodium ascorbate is added into colloidal solution A, is stirred continuously to being completely dissolved；
（3）Hydrogenperoxide steam generator is added, reductant solution is obtained after being uniformly mixed；
（4）The natural peach gums of 1.2 ~ 2.5kg are added in 30 ~ 60L deionized waters, disperses 1 ~ 2h, prepares colloidal solution B；
（5）Silver nitrate is added in colloidal solution B, obtains being reduced solution after stirring to its all dissolving；
（6）Solution will be reduced to be added in reductant solution, produced after the completion of reaction.
Embodiment 2：
The present embodiment optimizes the consumption and specific technological parameter of each composition：
（1）The natural peach gums of 10.0g are added in 200 sub- water, disperses 1h, prepares colloidal solution A；
（2）Colloidal solution A temperature is adjusted to 50 ~ 55 DEG C, 20.0kg sodium ascorbates are then added thereto, are stirred continuously
To being completely dissolved；
（3）Again to being dissolved with the colloidal solution A of sodium ascorbate, the hydrogen peroxide that 7.5L mass fractions are 20% is added
Solution, reductant solution is obtained after being uniformly mixed；
（4）The natural peach gums of 1.5kg are added in 53L deionized waters, disperses 1h, prepares colloidal solution B；
（5）20.0kg silver nitrates are added in colloidal solution B, obtain being reduced solution after stirring to its all dissolving；
（6）Solution will be reduced to be added in reductant solution with 0.25L/min speed, produced after the completion of reaction.
Gained silver powder particles size, such as Fig. 1, shown in Fig. 2, the physical property of gained silver powder see the table below,
Embodiment 3：
The present embodiment optimizes the consumption and specific technological parameter of each composition：
（1）The natural peach gums of 8.5kg are added in 200L deionized waters, disperses 1h, prepares colloidal solution A；
（2）Colloidal solution A temperature is adjusted to 50 ~ 55 DEG C, then thereto add 15kg sodium ascorbates, be stirred continuously to
It is completely dissolved；
（3）Again to being dissolved with the colloidal solution A of sodium ascorbate, the hydrogen peroxide that 5.0L mass fractions are 20% is added
Solution, reductant solution is obtained after being uniformly mixed；
（4）The natural peach gums of 1.2kg are added in 30L deionized waters, disperses 1h, prepares colloidal solution B；
（5）15kg silver nitrates are added in colloidal solution B, obtain being reduced solution after stirring to its all dissolving；
（6）Solution will be reduced to be added in reductant solution with 0.2L/min speed, produced after the completion of reaction.
Embodiment 4：
The present embodiment optimizes the consumption and specific technological parameter of each composition：
（1）The natural peach gums of 12.5kg are added in 350L deionized waters, disperses 2h, prepares colloidal solution A；
（2）Colloidal solution A temperature is adjusted to 50 ~ 55 DEG C, then thereto add 25kg sodium ascorbates, be stirred continuously to
It is completely dissolved；
（3）Again to being dissolved with the colloidal solution A of sodium ascorbate, the hydrogen peroxide that 9.5L mass fractions are 20% is added
Solution, reductant solution is obtained after being uniformly mixed；
（4）The natural peach gums of 2.5kg are added in 60L deionized waters, disperses 2h, prepares colloidal solution B；
（5）25kg silver nitrates are added in colloidal solution B, obtain being reduced solution after stirring to its all dissolving；
（6）Solution will be reduced to be added in reductant solution with 0.3L/min speed, produced after the completion of reaction.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that：Not
A variety of change, modification, replacement and modification can be carried out to these embodiments by departing under the principle and objective of the present invention, of the invention
Scope is limited by claim and its equivalent.
Claims (9)
1. a kind of high-dispersion submicron silver powder production method, it is characterised in that comprise the following steps：
(1) the natural peach gums of 8.5~12.5kg are added in 200~350L deionized waters, disperses 1~2h, prepares colloidal solution A；
(2) colloidal solution A temperature is adjusted to 45~60 DEG C, 15~25kg sodium ascorbates is then added thereto, are stirred continuously
To being completely dissolved；
(3) again to being dissolved with the colloidal solution A of sodium ascorbate, the peroxidating that 5.0~9.5L mass fractions are 20% is added
Hydrogen solution, reductant solution is obtained after being uniformly mixed；
(4) the natural peach gums of 1.2~2.5kg are added in 30~60L deionized waters, disperses 1~2h, prepares colloidal solution B；
(5) 15~25kg silver nitrates are added in colloidal solution B, obtain being reduced solution after stirring to its all dissolving；
(6) solution will be reduced to be added in reductant solution with 0.2~0.3L/min speed, is produced after the completion of reaction.
2. a kind of high-dispersion submicron silver powder production method according to claim 1, it is characterised in that the step (1)
In, the detailed process for preparing colloidal solution A is that the specific consumption of natural peach gum is 10.0kg, and the specific consumption of deionized water is
200L, jitter time is 1h.
3. a kind of high-dispersion submicron silver powder production method according to claim 1, it is characterised in that the step (2)
In, detailed process is that colloidal solution A temperature is adjusted into 50~55 DEG C, 20.0kg sodium ascorbates is then added thereto, not
Disconnected stirring is to being completely dissolved.
4. a kind of high-dispersion submicron silver powder production method according to claim 1, it is characterised in that the step (3)
In, the mass fraction of the hydrogenperoxide steam generator of addition is 20%, and it is 7.5L to add the amount of hydrogenperoxide steam generator.
5. a kind of high-dispersion submicron silver powder production method according to claim 1, it is characterised in that the step (1),
Step (2), the process of step (3) are carried out in 500L reactor.
6. a kind of high-dispersion submicron silver powder production method according to claim 1, it is characterised in that the step (4)
In, the detailed process for preparing colloidal solution B is that the specific consumption of natural peach gum is 1.5kg, and the specific consumption of deionized water is 53L,
Jitter time is 1h.
7. a kind of high-dispersion submicron silver powder production method according to claim 1, it is characterised in that the step (5)
In, it is necessary to add silver nitrate be 20kg.
8. a kind of high-dispersion submicron silver powder production method according to claim 1, it is characterised in that the step (4)
Process with step (5) is carried out in 100L reactor.
9. a kind of high-dispersion submicron silver powder production method according to claim 1, it is characterised in that the step (6)
In, solution will be reduced and be added to 0.25L/min speed in reductant solution.
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| CN102513546B (en) * | 2011-12-22 | 2013-09-18 | 广东羚光新材料股份有限公司 | Functional silver flake and preparation method thereof |
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| CN102764897B (en) * | 2012-08-09 | 2014-10-22 | 深圳市圣龙特电子有限公司 | Method for preparing submicron silver powder for electro-conductive paste |
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