CN110238385A - The preparation method of round pie chip super fine silver powder - Google Patents
The preparation method of round pie chip super fine silver powder Download PDFInfo
- Publication number
- CN110238385A CN110238385A CN201910708102.1A CN201910708102A CN110238385A CN 110238385 A CN110238385 A CN 110238385A CN 201910708102 A CN201910708102 A CN 201910708102A CN 110238385 A CN110238385 A CN 110238385A
- Authority
- CN
- China
- Prior art keywords
- solution
- silver powder
- preparation
- agno
- super fine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of preparation methods of round pie chip super fine silver powder, comprising the following steps: (1) ethylene glycol is heated to 170 DEG C, the temperature addition NaBr and polyvinylpyrrolidone for being kept for 170 DEG C are uniformly mixing to obtain solution I；(2) continue to keep solution I that AgNO is added in 170 DEG C of at a temperature of injection3AgNO is added in solution, injection3The process of solution keeps the stirring to solution I, with this condition AgNO3It reacts with ethylene glycol, AgNO3In Ag+It is reduced to obtain the silver of cube state, solution I becomes solution II at this time.The preparation method of round pie chip super fine silver powder of the invention, 170 DEG C at a temperature of, using polyvinylpyrrolidone as dispersing agent, while cooperating NaBr, the synergistic effect collective effect of the two make preparation silver powder become round pie chip particle, particle obtained uniformly and also good dispersion degree.Preparation method is simple, convenient for operation.
Description
Technical field
The present invention relates to silver powder preparation method technical field, in particular to a kind of preparation side of round pie chip super fine silver powder
Method.
Background technique
After functional material fine, when partial size is in micron, sub-micron and nano-scale, scale between atom,
Between molecule and bulk material, physicochemical properties are all varied widely, and are referred to as the 4th state of substance.With substance
Fine, surface molecular arrangement with electronic configuration distributed architecture and crystal structure all occurs it is corresponding change, produce
Peculiar small-size effect, skin effect, macro quanta tunnel effect and the quantum size effect that bulk material does not have, into
And make superfine powder compared with general large volume material, there is superior property in terms of physics, chemistry and interface, from
And it has an unexpected effect in application aspect.
Super fine silver powder is the silver powder of micron particle size, and particle shape has spherical, cotton-shaped, dendroid, rodlike, linear, vertical
Square shape, sheet and crystallite.The partial size of super fine silver powder is small, large specific surface area.This structure makes its fusing point year become smaller with particle and drop
Low, the interaction between atoms and electron spectrum of super fine silver powder surface atom have very big change with different inside silver powder
Activity is learned, therefore, when it is used on electronic component, the characteristics such as absorption related with surface, catalysis, diffusion, sintering are bright
Aobvious have dramatically different with large-sized silver powder, there is good electric conductivity.In addition, bulk effect (the i.e. volume of superfine function
Reduce, effect caused by the atom number reduction in particle) make it possible to the level spacing increasing with point, proton vibration and energy
Grade is discontinuous.It is active strong, it is easy to carry out various chemical reactions, there is very strong adsorption capacity and catalytic activity.Ultrafine particle
Surface there are many dangling bonds, there is unsaturated property, so as to cause the special adsorption phenomena and catalytic property of super fine silver powder.
The preparation method of super fine silver powder includes vapor phase method, solid phase method and liquid phase method.The investment of vapor phase method is big, energy consumption is high, produces
Rate is low；The silver powder partial size of solid phase method preparation is bigger than normal and particle size distribution range is wide；Liquid phase method technical process is fairly simple, powder
Grain size and shape is easy to control, and is that current low cost prepares the common method of silver powder.Have in the prior art much using liquid phase
The method that method prepares super fine silver powder, mainly using reducing agent such as glucose, hydrazine hydrate, boron Cymag, ascorbic acid etc. in liquid phase
Middle reduction silver salt solution obtains super fine silver powder, and silver powder obtained has spherical, dendroid etc., but in the prior art prepared by liquid phase method
Super fine silver powder dispersion degree it is poor, there are no prepare the report of round pie chip super fine silver powder, such as application number using chemical method
For the preparation method of 2015107269865 leaf shape silver powder.
Summary of the invention
In view of this, preparing round pie chip super fine silver powder using liquid phase reduction the purpose of the present invention is to provide a kind of
Method, silver powder good dispersion obtained, and particle diameter distribution is uniform.It is realized in particular by following technical scheme:
The preparation method of round pie chip super fine silver powder of the invention, comprising the following steps:
(1) ethylene glycol is heated to 170 DEG C, keeps 170 DEG C of temperature that NaBr and polyvinylpyrrolidone stirring is added
It is even to obtain solution I；
(2) continue to keep solution I that AgNO is added in 170 DEG C of at a temperature of injection3AgNO is added in solution, injection3The mistake of solution
Journey keeps the stirring to solution I, with this condition AgNO3It reacts with ethylene glycol, AgNO3In Ag+It is reduced to obtain cube
The silver of state, solution I becomes solution II at this time.
Further, further include step (3): after obtaining the silver of cube state for step (2), the solution II is at 25 DEG C
Cooling reaction, is then slowly added into acetone, is then centrifuged 10 minutes at 6000rpm, is cleaned with ethyl alcohol and removes impurity.
Further, the step (1) heats and keeps temperature to ethylene glycol using sand-bath.
Further, AgNO is added in injection in the step (2)3Injection rate be 5ml/h.
Further, the NaBr, polyvinylpyrrolidone and AgNO3Mass ratio be 71:500:266.
Beneficial effects of the present invention: the preparation method of round pie chip super fine silver powder of the invention, in 170 DEG C of temperature
Under, using polyvinylpyrrolidone as dispersing agent, while cooperating NaBr, the synergistic effect collective effect of the two makes preparation
Silver powder become round pie chip particle, particle obtained uniformly and also good dispersion degree.Preparation method is simple, convenient for operation.
Detailed description of the invention
The invention will be further described with reference to the accompanying drawings and examples:
Fig. 1 and Fig. 2 is the electron-microscope scanning figure using superfine cubic monocrystalline silver powder made from the method for the present invention.
Specific embodiment
The preparation method of round pie chip super fine silver powder in the present embodiment, first by the ethylene glycol of 40ml at 170 DEG C
In sand-bath heat 20min be heated to 170 DEG C, then keep 170 DEG C of temperature and stir under conditions of be added 28.4mgNaBr and
Polyvinylpyrrolidone (polyvinyl pyrrolidone, abbreviation PVP, use average molecular mass for 130000 it is poly-
Vinylpyrrolidone), stirring 30min obtains solution I.Take the analytically pure solid AgNO of 106.4mg3It dissolves in 1ml water and is formed
AgNO3Solution continues under conditions of keeping 170 DEG C of temperature and stirring in the AgNO for injecting preparation into solution with syringe pump3It is molten
Liquid, injection rate 5ml/h, with this condition AgNO3It reacts with ethylene glycol, AgNO3In Ag+It is reduced to obtain cake
The silver of shape chip, solution I becomes solution II at this time.After obtaining the silver of round pie chip, the cooling reaction at 25 DEG C of solution II, so
After be slowly added to acetone 2ml, be then centrifuged 10 minutes at 6000rpm, with ethyl alcohol clean remove impurity, repeated washing is until clear
Until wash clean.
During liquid-phase reduction prepares silver powder, need to overcome the agglomeration traits between the particle prepared.The group of powder
It is poly- to be primarily present in during two, one is the ultra-fine grain restored first is due to stirring heat fortune in reduction process
The factors such as dynamic collide with each other reunion together.Using polyvinylpyrrolidone as dispersing agent in the present invention, while cooperating NaBr,
The synergistic effect collective effect of the two makes the silver powder of preparation become the particle of round pie chip, and particle obtained is uniform and divides
Divergence is good, and as depicted in figs. 1 and 2, silver powder obtained is round pie chip, epigranular and good dispersion degree.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the scope of the claims of invention.
Claims (5)
1. a kind of preparation method of round pie chip super fine silver powder, it is characterised in that the following steps are included:
(1) ethylene glycol is heated to 170 DEG C, the temperature addition NaBr and polyvinylpyrrolidone for being kept for 170 DEG C are stirred evenly
To solution I；
(2) continue to keep solution I that AgNO is added in 170 DEG C of at a temperature of injection3AgNO is added in solution, injection3The process of solution is protected
The stirring to solution I is held, with this condition AgNO3It reacts with ethylene glycol, AgNO3In Ag+It is reduced to obtain a cube state
Silver, solution I becomes solution II at this time.
2. the preparation method of round pie chip super fine silver powder according to claim 1, it is characterised in that further include step
(3): after obtaining the silver of cube state for step (2), the solution II cooling reaction at 25 DEG C is then slowly added into third
Then ketone is centrifuged 10 minutes at 6000rpm, cleaned with ethyl alcohol and remove impurity.
3. the preparation method of round pie chip super fine silver powder according to claim 1, it is characterised in that: the step (1)
Temperature is heated and kept to ethylene glycol using sand-bath.
4. the preparation method of round pie chip super fine silver powder according to claim 1, it is characterised in that: the step (2)
AgNO is added in middle injection3Injection rate be 5ml/h.
5. the preparation method of round pie chip super fine silver powder according to claim 1, it is characterised in that: the NaBr, gather
Vinylpyrrolidone and AgNO3Mass ratio be 71:500:266.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910708102.1A CN110238385A (en) | 2019-08-01 | 2019-08-01 | The preparation method of round pie chip super fine silver powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910708102.1A CN110238385A (en) | 2019-08-01 | 2019-08-01 | The preparation method of round pie chip super fine silver powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110238385A true CN110238385A (en) | 2019-09-17 |
Family
ID=67893816
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910708102.1A Pending CN110238385A (en) | 2019-08-01 | 2019-08-01 | The preparation method of round pie chip super fine silver powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110238385A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102554258A (en) * | 2012-02-03 | 2012-07-11 | 济南大学 | Method for preparing metal silver nanostructure in water solution |
| CN102632246A (en) * | 2012-04-28 | 2012-08-15 | 苏州冷石纳米材料科技有限公司 | Method for preparing series silver nano-sheets in batch |
| CN103831444A (en) * | 2014-03-11 | 2014-06-04 | 上海交通大学 | Preparation method for high-crystallized flake silver powders |
| WO2016007942A1 (en) * | 2014-07-11 | 2016-01-14 | Northwestern University | Synthesis of uniform anisotropic nanoparticles |
| CN106735300A (en) * | 2016-12-22 | 2017-05-31 | 东南大学 | A kind of synthetic method of ultra-thin silver nanoparticle plate |
-
2019
- 2019-08-01 CN CN201910708102.1A patent/CN110238385A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102554258A (en) * | 2012-02-03 | 2012-07-11 | 济南大学 | Method for preparing metal silver nanostructure in water solution |
| CN102632246A (en) * | 2012-04-28 | 2012-08-15 | 苏州冷石纳米材料科技有限公司 | Method for preparing series silver nano-sheets in batch |
| CN103831444A (en) * | 2014-03-11 | 2014-06-04 | 上海交通大学 | Preparation method for high-crystallized flake silver powders |
| WO2016007942A1 (en) * | 2014-07-11 | 2016-01-14 | Northwestern University | Synthesis of uniform anisotropic nanoparticles |
| CN106735300A (en) * | 2016-12-22 | 2017-05-31 | 东南大学 | A kind of synthetic method of ultra-thin silver nanoparticle plate |
Non-Patent Citations (1)
| Title |
|---|
| 张丹慧，张成茂，杨厚波，邹文斌: "《贵金属/石墨烯纳米复合材料的合成及性能》", 31 December 2015, 国防工业出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110694616B (en) | Method for universally preparing load type metal monoatomic/metal nanoparticles | |
| CN102664275B (en) | Carbon-loaded kernel-shell copper-palladium-platinum catalyst for fuel battery and preparation method thereof | |
| CN102553579B (en) | Preparation method of high-dispersity supported nano metal catalyst | |
| CN110518257B (en) | Preparation method of carbon-supported transition metal @ Pt core-shell structure catalyst | |
| CN109935847A (en) | A kind of preparation method of the loaded platinum base alloy catalyst of low-temperature fuel cell | |
| CN105127441B (en) | A kind of preparation method of platinum nano microcrystalline dispersion | |
| CN101219378A (en) | Process for producing direct methanol fuel cell electro-catalyst | |
| Zheng et al. | Surfactant-free gold nanoparticles: rapid and green synthesis and their greatly improved catalytic activities for 4-nitrophenol reduction | |
| CN111451521A (en) | Method for preparing high-tap-density spherical silver powder by chemical method | |
| CN109482177A (en) | A kind of nano-noble metal catalyst preparation method | |
| CN104857955A (en) | Preparation method of noble metal nano catalyst | |
| CN109841856A (en) | A kind of preparation method of fuel cell monodisperse core-shell nano catalyst | |
| CN110238384A (en) | The preparation method of nanometer monocrystalline silver powder | |
| CN111640956A (en) | Method for preparing carbon-supported platinum electrocatalyst for fuel cell | |
| CN106179334A (en) | A kind of mesoporous carbon carried palladium catalyst and application thereof | |
| CN113707897A (en) | Anti-reversal catalyst for fuel cell and preparation method thereof | |
| CN109759049A (en) | A method of preparing the monatomic catalyst of mesoporous carbon-supported metal | |
| CN110756187A (en) | Gold-palladium/graphene catalyst growing on graphene surface in situ and preparation method thereof | |
| CN110238386A (en) | The preparation method of superfine cubic monocrystalline silver powder | |
| CN111940759A (en) | Method for preparing superfine platinum powder | |
| JP2019084491A (en) | Palladium core platinum shell fine particle colloid carried with carrier, palladium core platinum shell fine particle catalyst carried with carrier, manufacturing method therefor, and battery | |
| CN110238385A (en) | The preparation method of round pie chip super fine silver powder | |
| CN104259471A (en) | Method for preparing spherical silver nanoparticles uniform in particle size rapidly | |
| CN102211037A (en) | New method for preparing supported gold catalyst with anti-sintering property | |
| CN102133526A (en) | Method for preparing ruthenium carbon catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Shen Xianlin Inventor after: Hu Xiaobin Inventor after: Zhou Bin Inventor after: Mohammed Taher Inventor before: Hu Xiaobin Inventor before: Mohammed Taher Inventor before: Zhou Bin Inventor before: Shen Xianlin |
|
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190917 |