CN105880634B - A kind of preparation method of flaky nanometer silver powder - Google Patents
A kind of preparation method of flaky nanometer silver powder Download PDFInfo
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- CN105880634B CN105880634B CN201610515927.8A CN201610515927A CN105880634B CN 105880634 B CN105880634 B CN 105880634B CN 201610515927 A CN201610515927 A CN 201610515927A CN 105880634 B CN105880634 B CN 105880634B
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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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- 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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0551—Flake form nanoparticles
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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
- 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
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of flaky nanometer silver powder and preparation method thereof.This method is to heat to obtain mixed solution by silver salt, solvent and dispersant；Then alcohols reducing agent solution is added, pyroreaction obtains the mixed dispersion liquid of spherical nano-silver and flake nano silver；Finally use filter membrane circulating filtration, filter out spherical nano-silver, retention for flake nano silver, through being dried to obtain flaky nanometer silver powder.The particle of obtained flaky nanometer silver powder is triangular in shape, and thickness is 10 50nm, and size dimension is 100nm 500nm.Reaction system of the present invention is environmentally protective, and technical process is simple, and process costs are cheap, can realize that inexpensive mass prepares the flaky nanometer silver powder of even size distribution, even if reacting in higher concentrations, still can obtain flaky nanometer silver powder in high yield.
Description
Technical field
The invention belongs to noble metal nanometer material preparing technical field, and in particular in the solution using electronation legal system
The method of standby flaky nanometer silver powder.
Background technology
Metallic silver has excellent electric conductivity and thermal conductivity, widely should in fields such as printed electronic, catalysis, sensings
With.Research finds that the nano silver of different shape and size has different performance characteristics, therefore, carry out different sizes and pattern is received
Rice ag material synthesis is of great significance.
Since nano silver material has the advantages that particle is small, fusing point is low, anti-oxidant, electric conductivity is strong in printed electronic field
With important application, and flaky nanometer silver powder specific surface area is big and has a kind of special anisotropy nanostructured, this makes
Obtaining flake nano silver connectivity on film strengthens, i.e., electric conductivity is strong.Moreover, most long appearance and size reaches micron-sized
Shape nano-silver powder or a kind of more extreme anisotropy nanostructured, have great specific surface area and stronger anti-oxidant
Ability, is of great significance printed electronics field.
At present, in the report of flaky nanometer silver powder synthesis, reaction dissolvent is mostly organic solvent and reaction density is low, yield
Low (Shandong industrial technology, 2015,22,261), reaction process poor controllability (Rare Metal Materials and
Engineering, 2010,39,0401).
The content of the invention
The invention discloses a kind of flaky nanometer silver powder and preparation method thereof.This method be in water-based system, pass through by
Dihydric alcohol weak reductant solution is added dropwise to silver salt with being made in dispersant solution through pyroreaction.
The preparation method of the flaky nanometer silver powder is：Silver salt, solvent and dispersant are heated to obtain mix it is molten
Liquid；Then alcohols reducing agent is added, pyroreaction obtains the mixed dispersion liquid of spherical nano-silver and flake nano silver；Finally use
Filter membrane circulating filtration, filters out spherical nano-silver, retention for flake nano silver, through being dried to obtain flaky nanometer silver powder.
In parts by mass：The silver salt is 50-100 parts, solvent is 1000-2000 parts, dispersant is 100-200 parts,
Alcohols reducing agent is 150-250 parts, the solvent in alcohols reducing agent solution is 0-500 parts.
The silver salt is silver nitrate, the one or more in silver acetate, silver citrate, silver carbonate.
The solvent is water.
The dispersant is polyvinylpyrrolidone, polyvinyl alcohol, sodium citrate, Sodium Polyacrylate, polymethyl
One or more in sour sodium.
The Hybrid Heating temperature is -60 DEG C of room temperature.
The alcohols reducing agent is ethylene glycol, 1,3- propane diols, 1,2- propane diols, 1,2- butanediols, 1,3 butylene glycol
In one or more.
The pyroreaction temperature is 100-200 DEG C, when the reaction time is 1-3 small.
The aperture of the filter membrane is 100-200nm, preferably 150-200nm.
The drying temperature is 50-100 DEG C.
The diameter of the spherical nano-silver is less than 200nm.
The particle of the flaky nanometer silver powder is triangular in shape, thickness 10-50nm, size dimension 100nm-500nm.
The present invention is using water as reaction dissolvent, and alcohols is as reducing agent, and reaction system is environmentally protective, and technical process
Simply, process costs are cheap, can realize that inexpensive mass prepares the flaky nanometer silver powder of even size distribution, even in height
Reacted under concentration, still can obtain flaky nanometer silver powder in high yield.
Brief description of the drawings
Fig. 1 is the Electronic Speculum of the mixed dispersion liquid of the spherical nano-silver and flake nano silver obtained in 1 step of embodiment (2)
Figure.
Fig. 2 is the electron microscope of obtained flaky nanometer silver powder in 1 step of embodiment (3).
Fig. 3 is the electron microscope of obtained flaky nanometer silver powder in 2 step of embodiment (3).
Embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained all other without creative efforts
Embodiment, belongs to the scope of protection of the invention.
Embodiment 1
(1) in a 3L beaker, 0.9L secondary waters are added, after then adding the PVPK30 stirring and dissolvings of 60.0g, then are added
Enter 30.0g silver nitrates and continue stirring to dissolving, be eventually adding 0.1L ethylene glycol；
(2) solution obtained in step (1) is transferred in autoclave, at 120 DEG C and 400r/min mixing speeds
Lower reaction 2h, obtains the mixed dispersion liquid (such as Fig. 1) of spherical nano-silver and flake nano silver；
(3) mixed dispersion liquid obtained using the filter membrane of 100nm to step (2) carries out 5 filterings, will be trapped on filter membrane
Nano silver place 30min in 60 DEG C of baking oven and dry, that is, it be 10-50nm to obtain thickness, size dimension for 200-500nm piece
Shape nano-silver powder (such as Fig. 2).
Embodiment 2
(1) in a 3L beaker, 0.9L secondary waters are added, after then adding the PVPK30 stirring and dissolvings of 60.0g, then are added
Enter 30.0g silver nitrates and continue stirring to dissolving, be eventually adding the 1,3-PD of 0.15L；
(2) solution obtained in step (1) is transferred in autoclave, at 120 DEG C and 400r/min mixing speeds
Lower reaction 2.5h, obtains the mixed dispersion liquid of spherical nano-silver and flake nano silver；
(3) mixed dispersion liquid obtained using the filter membrane of 100nm to step (2) carries out 3 filterings, will be trapped on filter membrane
Nano silver place 30min in 60 DEG C of baking oven and dry, that is, it be 10-50nm to obtain thickness, size dimension for 200-500nm piece
Shape nano-silver powder (such as Fig. 3).
Embodiment 3
(1) in a 3L beaker, 0.9L secondary waters are added, after then adding the PVPK30 stirring and dissolvings of 60.0g, then are added
Enter 30.0g silver nitrates and continue stirring to dissolving, be eventually adding the 1,2-PD of 0.15L；
(2) solution obtained in step (1) is transferred in autoclave, at 150 DEG C and 400r/min mixing speeds
Lower reaction 2h, obtains the mixed dispersion liquid of spherical nano-silver and flake nano silver；
(3) mixed dispersion liquid obtained using the filter membrane of 100nm to step (2) carries out 5 filterings, will be trapped on filter membrane
Nano silver place 30min in 60 DEG C of baking oven and dry, that is, it be 10-50nm to obtain thickness, size dimension for 200-500nm piece
Shape nano-silver powder.
A kind of preparation method of the flaky nanometer silver powder provided above the embodiment of the present invention is described in detail, this
Specific case is applied in text to be set forth the principle of the present invention and embodiment, the explanation of above example is only intended to
Help to understand method and its core concept of the invention；Meanwhile for those of ordinary skill in the art, the think of according to the present invention
Think, in specific embodiments and applications there will be changes, in conclusion this specification content should not be construed as pair
The limitation of the present invention.
Claims (3)
1. a kind of preparation method of flaky nanometer silver powder, it is characterised in that its concrete operation step is：By silver salt, solvent and divide
Powder mixes, and room temperature to 60 DEG C of heating obtains mixed solution；Then alcohols reducing agent is added, 100-200 DEG C of pyroreaction 1-3 is small
When obtain the mixed dispersion liquid of spherical nano-silver and flake nano silver；Filter membrane circulating filtration is finally used, filters out spherical nano-silver,
Retention for flake nano silver, be dried to obtain flaky nanometer silver powder through 50-100 DEG C；Above-mentioned each raw material is in parts by mass：Described
Silver salt is 50-100 parts, solvent is 1000-2000 parts, dispersant is 100-200 parts, alcohols reducing agent is 150-250 parts；
The alcohols reducing agent is ethylene glycol, in 1,3- propane diols, 1,2- propane diols, 1,2- butanediols, 1,3 butylene glycol
It is one or more of；The aperture of the filter membrane is 200nm；The dispersant is polyvinylpyrrolidone, polyvinyl alcohol, lemon
One or more in sour sodium, Sodium Polyacrylate, sodium polymethacrylate；
The diameter of the spherical nano-silver is less than 200nm；The particle of the flaky nanometer silver powder is triangular in shape, and thickness is
10-50nm, size dimension 100nm-500nm.
2. preparation method according to claim 1, it is characterised in that the silver salt is silver nitrate, silver acetate, citric acid
One or more in silver, silver carbonate.
3. preparation method according to claim 1, it is characterised in that the solvent is water.
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| CN105880634B true CN105880634B (en) | 2018-05-04 |
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| CN106601368A (en) * | 2016-12-02 | 2017-04-26 | 天津宝兴威科技股份有限公司 | Method for preparing conducting film on substrate surface based on silver nanoparticle ink |
| CN106610144B (en) * | 2016-12-07 | 2019-10-25 | 桂林电子科技大学 | A kind of method that local surface plasma resonance absorption sunlight prepares steam |
| CN107377989A (en) * | 2017-06-21 | 2017-11-24 | 天津宝兴威科技股份有限公司 | A kind of preparation method of flaky nanometer silver powder |
| CN109290588B (en) * | 2018-11-08 | 2021-11-16 | 南京大学 | Preparation method of monodisperse triangular nano silver |
| CN110253033A (en) * | 2019-07-30 | 2019-09-20 | 三明学院 | A method of quickly preparing triangular silver nanosheet at room temperature |
| CN110819290B (en) * | 2019-11-29 | 2021-12-07 | 佛山市瑞福物联科技有限公司 | Preparation method of prepolymer containing nano silver sheets and conductive adhesive thereof |
| CN115805316A (en) * | 2021-09-14 | 2023-03-17 | 中国科学院化学研究所 | Flaky silver nanoparticles, preparation method thereof, conductive silver paste composition and conductive silver paste |
| CN113881100B (en) * | 2021-09-24 | 2023-04-25 | 深圳环能石墨烯科技有限公司 | Ag/Cu 2 O/rGO nano composite antibacterial agent, antibacterial master batch and preparation method thereof |
| CN115592125B (en) * | 2022-09-26 | 2024-02-02 | 昆明贵研新材料科技有限公司 | Preparation method of gold powder with coexistence of micron sheets and submicron particles |
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| US4435214A (en) * | 1981-10-02 | 1984-03-06 | Ercon, Inc. | Conductive compositions |
| CN1686646A (en) * | 2005-04-26 | 2005-10-26 | 四川大学 | Preparation method of grain size controllable single dispersed nano silver powder |
| CN102120265B (en) * | 2010-01-07 | 2013-04-10 | 中国科学院化学研究所 | Preparation method of colloid of mono-dispersed silver nano particles and nano silver powder and conductive ink thereof |
| CN102693772B (en) * | 2012-06-11 | 2016-01-20 | 清华大学深圳研究生院 | Flexible transparent conducting film and manufacture method thereof |
| CN104174864B (en) * | 2013-05-21 | 2016-06-01 | 中国科学院理化技术研究所 | The preparation method of a kind of nanometer or submicron order Argent grain powder |
| CN103722181B (en) * | 2014-01-21 | 2016-01-20 | 江苏欧耐尔新型材料有限公司 | Liquid phase reduction uses dispersant to prepare the method for nano-silver powder |
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