CN105880627B - A kind of preparation method for the micro silver powder for accurately controlling specific surface area - Google Patents
A kind of preparation method for the micro silver powder for accurately controlling specific surface area Download PDFInfo
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- CN105880627B CN105880627B CN201610316321.1A CN201610316321A CN105880627B CN 105880627 B CN105880627 B CN 105880627B CN 201610316321 A CN201610316321 A CN 201610316321A CN 105880627 B CN105880627 B CN 105880627B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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Abstract
The present invention relates to a kind of preparation method for the micro silver powder for accurately controlling specific surface area, comprise the following steps：(1) compound concentration is 0.5 1.5mol/L silver nitrate solution；(2) sodium carbonate liquor that concentration is 1.2 1.6mol/L is added dropwise into silver nitrate solution, adjusts pH to 10 13；(3) mass fraction is prepared as 0.05 0.1% polyvinyl alcohol and the mixed solution of gelatin；(4) mixed solution is well mixed with silver nitrate solution；(5) triethanolamine solution is instilled in silver nitrate solution, micro silver powder slurries is made；(6) by obtained micro silver powder slurry wash, filter, dry.The present invention is by controlling dispersant and protectant different ratio in silver powder reduction reaction, to realize to accurate control of the micro silver powder than surface agent；Its technique is simple, production cost is low, is suitable for industrially mass producing, and the micro silver powder of preparation is widely used in medium and high temperature sintering electric slurry.
Description
Technical field
The present invention relates to a kind of preparation method of micro silver powder, particularly a kind of micro silver powder for accurately controlling specific surface area
Preparation method.
Background technology
Metal ultrafine powder possesses superior catalytic performance, magnetic property, electrical property etc. in itself, thus Aero-Space, electronics,
Chemical and medicine industry, powder metallurgy etc. are in an increasingly wide range of applications.Wherein micro silver powder has good conduction and thermal conductivity,
It is widely used in electronics industry, as component and electrocondution slurry, conductive oils such as production piezoelectric ceramics, capacitor, potentiometers
The raw material of ink etc..It is increasing to the demand of electrocondution slurry with the development of electronics industry, while to the performance of electrocondution slurry
It is required that more and more higher.
The silver paste applied in the electronic components such as monopole ceramic capacitor, NTC, PTC, ZnO varistor is to sintering table
Sight brightness requirement is very high, has strict want to preparing the specific surface area size of silver powder, surface-active power needed for this kind of silver paste
Ask, silver powder specific surface area and surface-active can directly affect brightness and compactness after silver paste sintering film forming.In general, this
Kind silver powder specific surface area should be greater than 6m2/ g, has a stronger sintering activity, and this silver powder is referred to as slug type silver powder in specialty.In
State patent CN101972855A discloses a kind of high-temperature sintered silver paste micro silver powder preparation method, and it first prepares the silvering solution of colloidal sol shape
System, the reduction system of colloidal sol shape and protection solution, then three are mixed, by using sol-gal process and liquid phase chemical also
Former method is used cooperatively, and effective control has been carried out to course of reaction, the carry out industrialized production that can stablize, and ensures amplification production
Under still can homogeneous reaction, greatly improve reaction generation Argent grain pattern and other characterize homogeneity, ultimately generate flocculence
Soft-agglomerated silver powder, it is easy to collect the post processing such as washing；Reunion in course of reaction causes the specific surface area of micro silver powder to reduce.Song Xian
Just wait [Song Xiangang, Lou Hongtao, research [J] electronic components of specific surface area influence factor in the bright micro silver powders preparation process of beam
With material, 2013,32 (10), 29-32.], a kind of research of specific surface area influence factor in micro silver powder preparation process is disclosed,
Using solution phase chemical reduction, using hydrazine hydrate as reducing agent, polyvinylpyrrolidone (PVP) and gum arabic are dispersant,
Sodium carbonate is pH adjusting agent, has prepared the micro silver powder of high-specific surface area, research PVP dispersant dosages, silver-colored mass concentration, carbon
Influence of the factor such as sour sodium dosage, reaction temperature and cocurrent pressure to micro silver powder specific surface area, but the research not yet volume production so far
Change.
The slug type silver powder generally existing sintering activity of domestic preparation is poor at present, sintering shrinkage is big and compactness is poor etc.
Problem.For slug type micro silver powder, specific surface area is higher, and sintering activity is stronger, it is desirable to sintering temperature it is lower, can realize preferably
Grain boundary decision, its silver layer surface glossiness and compactness after sintering is relatively good.Accordingly, it is capable to no prepare high-ratio surface
Long-pending micro silver powder decides the quality of made face electrodes conduct silver paste performance.
The content of the invention
To solve the above problems, deficiency of the object of the invention aiming at prior art, there is provided one kind is by controlling silver powder
Dispersant and protectant different ratio in reduction reaction, the preparation method for the micro silver powder for accurately controlling specific surface area is realized,
Its technique is simple, production cost is low, is easy to volume production, is suitable for industrially mass producing, and the granularity of the micro silver powder of preparation is
0.1-8.0 μm, specific surface area 1.0-8.0m2/ g, it is widely used in medium and high temperature sintering electric slurry.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of preparation method for the micro silver powder for accurately controlling specific surface area, comprises the following steps：
(1) silver nitrate solution is prepared with deionized water, the concentration of silver nitrate is 0.5-1.5mol/L in solution；
(2) sodium carbonate liquor that concentration is 1.2-1.6mol/L, regulation are added dropwise in the silver nitrate solution prepared to step (1)
PH to 10-13, stirred with 80r/mim rotating speed；
(3) polyene ethanol and gelatin mixed-powder are inserted in the deionized water that temperature is 80 DEG C, stirs 1-2h, obtain matter
Fraction is measured as 0.05-0.1% polyvinyl alcohol and the mixed solution of gelatin, the wherein mass ratio of polyvinyl alcohol and gelatin is 1-
10:5；
(4) mixed solution of step (3) is added in the silver nitrate solution of step (2), stirred with 60r/min rotating speed
Mix well mixed；
(5) triethanolamine solution is instilled in the silver nitrate solution of step (4) with 0.5-1mL/min speed, silver is made
Micro mist slurries；
(6) by micro silver powder slurry wash made from step (5), filtering, after the wet micro silver powder obtained after filtering is dried, obtain
Micro silver powder.
Specifically, the mass ratio of polyvinyl alcohol and gelatin is 2-8 in the step (3):5.
Specifically, polyvinyl alcohol quality is the 0.1%-0.3% of silver nitrate solid masses in the step (4).
Specifically, the ratio between amount of material of triethanolamine and silver nitrate is (1.5-5) in the step (5):1.
Specifically, the step (2), (4), the constant system reaction temperature of (5) are 25-40 DEG C.
Specifically, the granularity for the micro silver powder that the step (5) obtains is 0.1-8.0 μm, specific surface area 1.0-8.0m2/
g。
The present invention has beneficial effect：
(1) present invention is micro- to silver to realize by controlling dispersant and protectant different ratio in silver powder reduction reaction
The accurate control of powder specific surface area, specific surface area can be controlled in 1.0-8.0m2/g。
(2) preparation method of the present invention has that technique is simple, production cost is low, is easy to volume production, is suitable for industrial extensive
Production, the granularity of the micro silver powder prepared is 0.1-8.0 μm.
(3) micro silver powder prepared by the present invention is well mixed according to a certain percentage, and preferable sintering effect can be achieved, and is had good
The advantages that uniformity, solderability, soldering resistance, electric conductivity and the surface smoothness of good film layer, brightness.
Embodiment
Presently in connection with embodiment, the present invention is further detailed explanation.
Embodiment 1
A kind of preparation method for the micro silver powder for accurately controlling specific surface area, comprises the following steps：
(1) silver nitrate solution is prepared with deionized water, the concentration of silver nitrate is 0.5mol/L in solution；
(2) to step (1) prepare silver nitrate solution in be added dropwise concentration be 1.2mol/L sodium carbonate liquor, regulation pH to
12, stirred with 80r/mim rotating speed；
(3) it is 1 by mass ratio:5 polyene ethanol and gelatin mixed-powder are inserted in the deionized water that temperature is 80 DEG C, are stirred
1-2h is mixed, obtains mass fraction as 0.1% polyvinyl alcohol and the mixed solution of gelatin；
(4) mixed solution of step (3) is added in the silver nitrate solution of step (2), stirred with 60r/min rotating speed
Mix it is well mixed, wherein polyvinyl alcohol quality be silver nitrate solid masses 0.2%；
(5) triethanolamine solution is instilled in the silver nitrate solution of step (4) with 0.8mL/min speed, it is micro- that silver is made
The ratio between amount of material of slurry liquid, wherein triethanolamine and silver nitrate is 3:1；
Wherein, step (2), (4), the constant system reaction temperature of (5) are 25-40 DEG C
(6) by micro silver powder slurry wash made from step (5), filtering, after the wet micro silver powder obtained after filtering is dried, obtain
Micro silver powder, average grain diameter are 5-8 μm, specific surface area 1-1.8m2/ g, in light gray, purity >=99.9%.
Embodiment 2-11 and scheme other conditions with embodiment 1, difference such as following table：
It is complete by above-mentioned description, relevant staff using the above-mentioned desirable embodiment according to the present invention as enlightenment
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to determines its technical scope according to right.
Claims (7)
1. a kind of preparation method for the micro silver powder for accurately controlling specific surface area, comprises the following steps：
(1) silver nitrate solution is prepared with deionized water, the concentration of silver nitrate is 0.5-1.5mol/L in solution；
(2) to step (1) prepare silver nitrate solution in be added dropwise concentration be 1.2-1.6mol/L sodium carbonate liquor, regulation pH to
10-13, stirred with 80r/mim rotating speed；
(3) polyene ethanol and gelatin mixed-powder are inserted in the deionized water that temperature is 80 DEG C, stirs 1-2h, obtain quality point
Number is 0.05-0.1% polyvinyl alcohol and the mixed solution of gelatin, and the wherein mass ratio of polyvinyl alcohol and gelatin is 1-10:
5；
(4) mixed solution of step (3) is added in the silver nitrate solution of step (2), be stirred with 60r/min rotating speed
Uniformly；
(5) triethanolamine solution is instilled in the silver nitrate solution of step (4) with 0.5-1mL/min speed, micro silver powder is made
Slurries；
(6) by micro silver powder slurry wash made from step (5), filtering, after the wet micro silver powder obtained after filtering is dried, obtain silver-colored micro-
Powder.
2. the preparation method of the micro silver powder as claimed in claim 1 for accurately controlling specific surface area, it is characterised in that：The step
Suddenly the mass ratio of polyvinyl alcohol and gelatin is 2-8 in (3):5.
3. the preparation method of the micro silver powder as claimed in claim 1 for accurately controlling specific surface area, it is characterised in that：The step
Suddenly polyvinyl alcohol quality is the 0.1%-0.3% of silver nitrate solid masses in (4).
4. the preparation method of the micro silver powder as claimed in claim 1 for accurately controlling specific surface area, it is characterised in that：The step
Suddenly the ratio between amount of material of triethanolamine and silver nitrate is (1.5-5) in (5):1.
5. the preparation method of the micro silver powder as claimed in claim 1 for accurately controlling specific surface area, it is characterised in that：The step
Suddenly (2), (4), the constant system reaction temperature of (5) are 25-40 DEG C.
6. the preparation method of the micro silver powder as claimed in claim 1 for accurately controlling specific surface area, it is characterised in that：The step
Suddenly the granularity for the micro silver powder that (6) obtain is 0.1-8.0 μm.
7. the preparation method of the micro silver powder as claimed in claim 1 for accurately controlling specific surface area, it is characterised in that：The step
Suddenly the specific surface area for the micro silver powder that (6) obtain is 1.0-8.0m2/g。
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| CN107866562B (en) * | 2017-12-15 | 2019-09-06 | 湖南纳科新材料科技有限公司 | A kind of spherical golden micro mist and its preparation method and application |
| CN110355380B (en) * | 2019-08-13 | 2022-06-28 | 山东建邦胶体材料有限公司 | Preparation method of hexagonal flaky micron-crystal silver powder |
| CN112008094B (en) * | 2020-09-08 | 2024-03-01 | 西安汇创贵金属新材料研究院有限公司 | Silver powder preparation method |
| CN113290252A (en) * | 2021-05-28 | 2021-08-24 | 金川集团股份有限公司 | Preparation method of superfine silver powder with low tap mass and high specific surface |
| CN114054769B (en) * | 2021-11-17 | 2024-05-03 | 广东羚光新材料股份有限公司 | Silver micro powder and preparation method and application thereof |
| CN114850480B (en) * | 2022-05-28 | 2023-09-19 | 中船黄冈贵金属有限公司 | Preparation method of high-conductivity flake silver powder for touch screen silver paste |
| CN116741480A (en) * | 2023-06-05 | 2023-09-12 | 肇庆市金龙宝电子有限公司 | NTC thermistor based on gold electrode sintering and preparation method thereof |
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| CN101733410B (en) * | 2009-12-31 | 2013-05-01 | 广东风华高新科技股份有限公司 | Preparation method of high dispersibility superfine silver powder with adjustable grain diameter |
| CN103143723B (en) * | 2013-03-27 | 2015-09-30 | 深圳市中金岭南科技有限公司 | A kind of method preparing the flake silver powder of low-apparent-density |
| JP6029720B2 (en) * | 2014-07-31 | 2016-11-24 | Ｄｏｗａエレクトロニクス株式会社 | Silver powder, method for producing the same, and conductive paste |
| CN104084598A (en) * | 2014-08-01 | 2014-10-08 | 天津市职业大学 | Production method for solar cell high-density monodisperse silver powder |
| CN104190946B (en) * | 2014-08-29 | 2016-04-13 | 广东风华高新科技股份有限公司 | The preparation method of high-tap density surface modification silver powder |
| CN104325151A (en) * | 2014-10-11 | 2015-02-04 | 中国振华集团云科电子有限公司 | Silver powder preparing method |
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