CN110919025A - Preparation method of nano paillette silver powder - Google Patents
Preparation method of nano paillette silver powder Download PDFInfo
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- CN110919025A CN110919025A CN201911224686.1A CN201911224686A CN110919025A CN 110919025 A CN110919025 A CN 110919025A CN 201911224686 A CN201911224686 A CN 201911224686A CN 110919025 A CN110919025 A CN 110919025A
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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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention belongs to the technical field of nano material preparation, and particularly relates to a method for preparing nano paillette silver powder in an alcohol-water mixed system. The method is a method for preparing the nano paillette silver powder by a liquid phase chemical reduction method in an alcohol/water mixed system, and has the advantages of short reaction time, high efficiency, simple process and equipment, green and environment-friendly used reagents, low cost and particular suitability for batch production; the nano paillette silver powder has irregular flake shape, smooth surface, clear boundaries between flakes, thickness of 40-70nm, flake diameter less than or equal to 30 microns and silver content greater than 99.8%. In addition, the nano paillette silver powder has sintering activity at 206.7 ℃, can be partially sintered, and has less carbon residue after low-temperature sintering.
Description
Technical Field
The invention relates to the technical field of preparation of nano flaky silver powder; in particular to a method for preparing nano paillette silver powder in an alcohol-water mixed system.
Background
With the development of microelectronic devices, high-frequency high-power packaging technology has become more and more important in the field of electronic packaging as a key core technology. Research shows that the nano silver powder with low-temperature sinterability is a novel connecting material for replacing traditional interface connecting materials such as brazing filler metal, lead-free brazing filler metal, heat-conducting glue, conducting resin and the like, and has very important influence on the development of electronic devices and circuits. The nano flaky silver powder with the flexible planar structure can establish a conductive path or a heat conduction path through line contact or surface contact, and compared with spherical nano silver powder, the joint has better electrical conductivity and thermal conductivity. Therefore, the nano flaky silver powder can be widely applied to the fields of electronic paste, conductive adhesive, electromagnetic shielding, semiconductor chip packaging and the like, and has great application value.
At present, the preparation method of the nano flaky silver powder mainly comprises a reduction ball milling method, a catalytic reduction method, a photoinduction method, a seed crystal method, a template method, a hydrothermal method, an electrochemical synthesis method and the like. The methods such as the photoinduction method, the template method, the hydrothermal method, the electrochemical synthesis method and the like have high cost, low yield and long time, and only micro-synthesis can be carried out; the reduction ball milling method, the catalytic reduction method, the seed crystal method and the like have higher synthesis efficiency, but the synthesized nano flaky silver powder has smaller sheet diameter which is mostly 100-500 nm.
28/2014, 05 and 28, and chinese patent publication (publication) No. CN103817346A, disclose hu xiao et al to propose a preparation method of a morphology-controllable triangular flaky nano silver powder, which induces trisodium citrate to reduce a silver nitrate aqueous solution to synthesize the triangular flaky nano silver powder by reducing an initiator sodium borohydride to generate crystal nuclei, wherein the flaky silver powder has a sheet diameter of less than 50 nm.
24/2016, and the Chinese patent publication (publication) No. CN105880634A of invention discloses a preparation method of flake nano silver powder proposed by Zhang xing industry, etc., which comprises reducing silver salt at high temperature under the condition of 100 plus materials and 120 ℃ by alcohol reducing agent to obtain a mixed dispersion of spherical nano silver and flake nano silver, and finally filtering by adopting a filter membrane to filter out spherical nano silver, wherein the trapped flake nano silver is obtained, and the nano silver powder particles are triangular, have the thickness of 10-50nm and the side length of 100 plus materials and 500 nm.
In 2018, 08 and 17 months, China invention patent publication (publication) No. CN108405869A discloses a method for preparing flake silver powder with small particle size, which is disclosed by CaoDu et al, and the like, and the flake silver powder with small particle size, with the average particle size of 3-7 microns and the tap density of 3.0-5.0g/cm3 nanometer-scale thickness, is prepared by ball milling high-dispersity silver powder with the silver content of more than 99.95 percent and the particle size of 2-3 microns.
20/03/2013, and chinese patent publication (publication) No. CN102974839A, disclose methods for preparing nano-sized silver flakes by chemical deposition, such as chen zheng xing, and the like, by depositing a nano-sized silver film on the surface of a soluble resin substrate, dissolving the substrate by an organic solvent, and ultrasonically crushing to obtain the nano-sized silver flakes.
2019, 03 month 08, China invention patent publication (Notification) No. CN109434131A, discloses a method for preparing nano-silver powder in flake form by yili pine and the like, and adopts hydrothermal method to prepare precursor Ag3C2O4The large-area flaky nano silver powder is prepared by thermal decomposition, the thickness of the flaky nano silver powder is between 35nm and 60nm, the flaky nano silver powder is mostly triangular and slightly flaky, and the side length is about 5 mu m.
In addition, organic high molecular polymers or organic macromolecules can be added in the synthesis process of the nano flaky silver powder as dispersing agents (such as polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), polyethylene glycol (PEG), polyacrylic acid (PAA), sodium hexadecylsulfonate (CTAB) and the like) to control the morphology of the nano flaky silver powder, the dispersibility of the nano flaky silver powder is improved, and the prepared silver powder often contains more organic matter residues. The macromolecular organic matters have higher decomposition temperature, low solubility and large difficulty in cleaning and removing, and have the problems of system phase tolerance, performance reduction and the like in the using process.
24/2011 08/month and 24/month, chinese patent publication (publication) No. CN109434131A, discloses chaiheiyuan, etc. to provide a micron-sized flaky nano silver powder and a preparation method thereof, wherein an interface method is adopted, phenylenediamine is adopted to reduce silver nitrate at a benzene/water solution interface to prepare the micron-sized flaky nano silver powder, the longest dimension of the obtained flaky nano silver powder particles is between 10 and 30 μm, the flaky nano silver powder particles are in a saw-tooth shape, and the surfaces of the flaky nano silver powder particles are wrapped by a poly-p-phenylenediamine molecular layer with the thickness of less than 10 nm.
2016, month 01 and month 27, and Chinese patent publication (publication) No. CN105268993A, disclose a method for preparing flaky nano silver powder from Lizhongchun, which comprises reducing silver salt solution containing surfactant (polyvinylpyrrolidone PVP-k 30) with ferrous salt solution at 40-100 deg.C to obtain flaky nano silver powder particles with 5-10 μm sheet diameter.
Therefore, the method has important significance and wide market prospect for preparing the nano flaky silver powder in a batch manner with high efficiency, green, low cost and by selecting a proper reaction system, a proper dispersant (protective agent) and other additives.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of nano paillette silver powder; the method has the advantages of high efficiency, greenness, low cost and easy realization of industrialization, and the prepared nano paillette silver powder has certain low-temperature sintering activity.
In order to realize the purpose, the invention adopts the technical scheme that:
a preparation method of nano paillette silver powder comprises the following steps:
(1) weighing 8.5g silver nitrate (AgNO)3) Taking a proper amount of alcohol/water mixed solution to dissolve AgNO as raw materials under the condition of constant temperature stirring3Preparation of AgNO3Alcohol/water solution with concentration of 0.05-0.5 mol/L; then, a proper amount of dispersant is weighed and dissolved in the prepared AgNO3Stirring the mixture evenly in an alcohol/water solution to obtain a reaction solution A;
(2) under the condition of constant-temperature stirring, taking a proper amount of alcohol/water mixed solution to dissolve a reducing agent, wherein the concentration is 0.5-2mol/L, and obtaining a reaction solution B;
(3) quickly pouring the reaction solution B prepared in the step (2) into the reaction solution A prepared in the step (1) under the condition of constant-temperature high-speed stirring, and quickly and uniformly mixing to obtain a slightly milky reaction solution;
(4) after the solution components in the step (3) are uniformly mixed, adding 100-200mLNH into the reaction solution under the condition of constant temperature and high speed stirring3·H2O, changing the slightly milky white reaction solution into a light yellow brown transparent solution;
(5) dissolving 8-15g of NaOH by using a proper amount of alcohol/water mixed solution, wherein the concentration is 1-3 mol/L; pouring the prepared NaOH alcohol/water solution into the reaction solution in the step (4), fully stirring at constant temperature, and changing the color of the solution from light tan to dark brown;
(6) dissolving 3-6g of glycolic acid with a proper amount of alcohol/water mixed solution, wherein the concentration is 1-3 mol/L; then pouring the prepared ethanol/water solution of the ethanol into the reaction solution in the step (4), fully stirring at constant temperature for 5-10min, and changing the color of the solution from dark brown to black transparent solution;
(7) placing the black transparent solution in the step into an oven (or a constant-temperature water bath kettle), standing for 1-3h at a constant temperature under the condition of 30-50 ℃, and carrying out reduction reaction; during the standing process, the generation of the paillette product can be seen by naked eyes, the solution is settled, and the color of the solution is gradually changed into yellow green transparent solution from black transparent solution;
(8) after the reduction reaction is finished, removing the supernatant in the step (6), and then centrifugally separating the bottom suspension at the rotation speed of 3000-;
(9) adding the flake silver powder (crude product) obtained in the step (8) into a certain amount of pure water, and continuously stirring for 10-30min under the condition that the rotating speed is 1000-3000 r/min; then standing for 30-60min, and then centrifugally separating the flaky silver powder sample and the cleaning waste liquid under the condition that the rotating speed is 3000-;
(10) adding the flake silver powder sample obtained in the step (9) into a certain amount of ethanol/pure water mixed solution, and continuously stirring for 10-120min under the condition that the rotating speed is 1000-3000 r/min; then standing for 30-60min, and then centrifugally separating the flaky silver powder sample and the cleaning waste liquid under the condition that the rotating speed is 3000-;
(11) adding the flake silver powder sample obtained in the step (10) into a certain amount of absolute ethyl alcohol, and continuously stirring for 10-120min under the condition that the rotating speed is 1000-3000 r/min; then standing for 30-60min, and then centrifugally separating the flaky silver powder sample and the cleaning waste liquid under the condition that the rotating speed is 3000-;
(12) and (3) drying the silver powder slurry obtained in the step (11) into the nano paillette silver powder in a vacuum drying mode at the temperature of 60-80 ℃.
The specific technical scheme of the invention also comprises:
(1) the alcohol/water mixed solution used in the invention is a mixed solution obtained by mixing absolute ethyl alcohol and deionized water according to a certain proportion, and the mixing proportion of the absolute ethyl alcohol and the deionized water is as follows: 1:1-3: 1;
(2) the dispersants (protective agents) used in the present invention are: hydrogenated rosin alcohol; the dosage of the dispersant is 30 to 50 percent of the theoretical silver powder yield (mass);
(3) the reducing agent used in the invention is: one or two of triethanolamine and ethylene glycol;
(4) the amounts of the reaction solution A and the reaction solution B used in the present invention were determined according to AgNO3Molar ratio to reducing agent, and M (AgNO)3): m (reducing agent) is 1 (1.5-3);
(5) AgNO in the invention3And the stirring speed when the reducing agent is dissolved is as follows: 1000-2000r/min, the temperature is: 30-60 ℃;
(6) the stirring speed when the reaction solution A and the reaction solution B are mixed is as follows: 2000-4000r/min, and the constant temperature is as follows: 30-60 ℃;
(7) in the invention, the reaction residual liquid after the reduction reaction can be recovered and returned to a smelting system to re-extract the metallic silver; the alcohol-containing waste liquid in the cleaning process can be used for recovering ethanol in a distillation mode and reusing the ethanol.
The nano paillette silver powder has irregular flake shape, smooth surface, clear boundary between flakes, thickness of 40-70nm, flake diameter less than or equal to 30 mu m and silver content more than 99.8 percent; the nano paillette silver powder can be partially sintered within the range of 200-; after being dried, the nano paillette silver powder is observed by naked eyes to be in a bright silver color.
The invention has the beneficial effects that:
(1) the large-sheet-diameter nano paillette silver powder is prepared by adopting a liquid-phase chemical reduction method in an alcohol/water mixed system, the thickness of the flaky nano silver powder is between 40nm and 70nm, the sheet diameter is less than or equal to 30 mu m, the reaction time is short, the efficiency is high, the process and the equipment are simple, and the method is particularly suitable for batch production;
(2) the surface of the nano paillette silver powder is smooth and flat, and ideal surface contact or line contact is easy to form, so that the nano paillette silver powder is particularly suitable for being applied to the fields of electric conduction and heat conduction;
(3) the reducing agent used in the invention is triethanolamine and ethylene glycol weak reducing agent, the reaction process is mild and easy to control; secondly, hydrogenated rosin alcohol is used as a dispersing agent (or a protective agent), the molecular weight is small, the solubility is high, the cleaning is easy, the purity of the prepared nano paillette silver powder is high, the dispersibility is good, and the dried powder is in a paillette silver white color;
(4) the additive or the reaction auxiliary agent used in the invention is a conventional agent, is green and environment-friendly, and has low cost;
(5) the reduction reaction residual liquid can be recovered and returned to the smelting system, so that silver is recovered, and waste is reduced; the alcohol-containing waste liquid in the cleaning process can be used for recovering the ethanol in a distillation mode, so that the utilization rate of the ethanol is improved.
Drawings
Fig. 1 is a photograph of a dried sample of nano spangle silver powder.
Fig. 2 is an SEM image of the nano spangle silver powder prepared in example one.
FIG. 3 is DSC and TGA curves of the nano spangle silver powder prepared in the first example.
Detailed Description
The first embodiment is as follows:
a preparation method of nano paillette silver powder comprises the following steps:
(1) weighing 8.5g silver nitrate (AgNO)3) Taking a proper amount of alcohol/water mixed solution to dissolve AgNO as raw materials under the condition of constant temperature stirring3Preparation of AgNO3Alcohol/water solution with concentration of 0.1mol/L (wherein the mixing ratio of the absolute ethyl alcohol and the deionized water is 2: 1); then, hydrogenated rosin having a theoretical yield (mass) of 30% of silver powder was weighed outAlcohol dispersant and dissolved in prepared AgNO3Stirring the mixture evenly in an alcohol/water solution to obtain a reaction solution A; and the dissolving process is kept at the constant temperature of 40 ℃, and the stirring speed is as follows: 1000 r/min;
(2) under the condition of constant-temperature stirring, dissolving 12g of reducer triethanolamine in alcohol/water mixed solution to prepare 0.8mol/L triethanolamine reduction solution to obtain reaction solution B, wherein the temperature of the reducer dissolving process is constant at 40 ℃, and the stirring speed is as follows: 1000 r/min;
(3) at a constant temperature of 40 ℃, the stirring speed is as follows: quickly pouring the reaction solution B prepared in the step (2) into the reaction solution A prepared in the step (1) under the condition of 3000r/min, and quickly and uniformly mixing to obtain a slightly milky reaction solution;
(4) after the solution components in the step (3) are uniformly mixed, adding 120mLNH into the reaction solution under the condition of constant temperature and high-speed stirring3·H2O, changing the slightly milky white reaction solution into a light yellow brown transparent solution;
(5) weighing 10g of NaOH and dissolving in a proper amount of alcohol/water mixed solution, wherein the concentration is 1 mol/L; pouring the prepared NaOH alcohol/water solution into the reaction solution in the step (4), fully stirring at constant temperature, and changing the color of the solution from light tan to dark brown;
(6) weighing 4g of glycollic acid, and dissolving the glycollic acid in a proper amount of alcohol/water mixed solution, wherein the concentration is 2 mol/L; then pouring the prepared ethanol/water solution of the glycolic acid into the reaction solution in the step (4), and continuously stirring for 10min under the conditions of constant temperature of 40 ℃ and 3000r/min, wherein the color of the solution is changed from dark brown to black transparent solution;
(7) placing the black transparent solution in the step into an oven (or a constant-temperature water bath kettle), standing for 2 hours at a constant temperature under the condition of 40 ℃, and carrying out reduction reaction; during the standing process, the generation of the paillette product can be seen by naked eyes, the solution is settled, and the color of the solution is gradually changed into yellow green transparent solution from black transparent solution;
(8) after the reduction reaction is finished, removing the supernatant in the step (6), and then centrifugally separating the bottom suspension at the rotation speed of 4000r/min to obtain the flaky silver powder (crude product) and reaction residual liquid;
(9) adding the flake silver powder (crude product) obtained in the step (8) into a certain amount of pure water, and continuously stirring for 15min under the condition that the rotating speed is 2000 r/min; then standing for 30min, and then centrifugally separating the flaky silver powder sample and the cleaning waste liquid under the condition that the rotating speed is 4000 r/min;
(10) adding the flake silver powder sample obtained in the step (9) into a certain amount of ethanol/pure water mixed solution, and continuously stirring for 15min under the condition that the rotating speed is 2000 r/min; then standing for 30min, and then centrifugally separating the flaky silver powder sample and the cleaning waste liquid under the condition that the rotating speed is 4000 r/min;
(11) adding the flake silver powder sample obtained in the step (10) into a certain amount of absolute ethyl alcohol, and continuously stirring for 150min under the condition that the rotating speed is 2000 r/min; then standing for 30min, and then centrifugally separating the flaky silver powder sample and the cleaning waste liquid under the condition that the rotating speed is 4000 r/min;
(12) drying the silver powder slurry obtained in the step (11) into nano paillette silver powder in a vacuum drying mode at the temperature of 70 ℃;
FIG. 1 is a photograph of a dried sample of the nano spangle silver powder prepared in example one, and it can be seen from the photograph that the nano spangle silver powder prepared by the present invention is bright silver after being dried, and has uniform color and luster, which indicates that the silver powder has large flake diameter, good crystallinity and high silver content; FIG. 2 is a Scanning Electron Microscope (SEM) spectrum of the nano paillette silver powder prepared in the first embodiment, and it can be seen that the thickness of the lamella of the nano paillette silver powder prepared by the invention is between 40 and 70nm, the diameter of the lamella is less than or equal to 30 μm, and the area of the single lamella is much larger than that of the nano paillette silver powder prepared by other methods; in addition, as can be seen from the figure, the surface of the nano paillette silver powder is smooth, the boundary between the sheets is clear, the crystallinity is good, and the silver powder has good dispersibility. Fig. 3 is a Differential Scanning Calorimetry (DSC) and thermogravimetric analysis (TGA) curve of the nano spangle silver powder prepared in the first example. It can be seen from the thermogravimetric analysis curve that the silver content of the nano spangle silver powder prepared by the invention is 98.84%, the organic compound containing 1.16% exists, probably because a small amount of dispersant molecules are adsorbed on the surface of the nano spangle silver powder in the synthesis process and a small amount of silver-containing compound is included in the nano spangle silver powder, and when the temperature is higher than 300 ℃, only 0.204% of impurities remain. In addition, as can be seen from FIG. 3, the endothermic peak of the silver nanoparticle at 206.7 ℃ is shown, and the weight change is small, which indicates that the silver nanoparticle is in a melting and sintering state at the time, and the sintering temperature is far lower than the melting temperature of the metallic silver (961 ℃), and the silver nanoparticle can be applied to the field of low-temperature sintering.
Claims (9)
1. A method for preparing nano paillette silver powder is characterized by comprising the following steps:
mixing silver nitrate and a hydrogenated rosin alcohol dispersing agent in an alcohol/water mixed solution to obtain a silver nitrate dispersed solution, wherein the alcohol/water mixed solution is a mixed solution of absolute ethyl alcohol and deionized water; quickly adding a reducing agent solution into a silver nitrate dispersion solution, quickly mixing, and carrying out reduction reaction to obtain a reaction solution, wherein the reducing agent is one or two of triethanolamine or ethylene glycol, and the molar ratio of silver nitrate to the reducing agent is 1 (1.5-3); then respectively adding ammonia water, sodium hydroxide and glycolic acid into the reaction solution, mixing, reacting, and standing for 1-3 hours to obtain a silver powder suspension; and centrifugally separating and drying to obtain the nano paillette silver powder.
2. The method for preparing nano spangle silver powder according to claim 1, wherein the reaction system is an alcohol/water mixed system, and the alcohol/water mixed solution is a mixed solution of absolute ethyl alcohol and deionized water, and the mixing ratio of the absolute ethyl alcohol to the deionized water is as follows: 1:1-3:1.
3. The method for preparing nano spangle silver powder according to claim 1, wherein the reducing agent is one or two of triethanolamine or ethylene glycol, and AgNO3The mol ratio of the reducing agent to the reducing agent is 1 (1.5-3).
4. The method for preparing nano spangle silver powder according to claim 1, wherein the dispersant is hydrogenated abienol, and the weight of the dispersant is 30-50% of the theoretical silver powder weight.
5. The method for preparing nano spangle silver powder according to claim 1, wherein ammonia, sodium hydroxide and glycolic acid are added in the reaction process.
6. The method for preparing nano spangle silver powder according to claim 1, wherein the reaction solution is uniformly mixed and then kept at a constant temperature within a range of 30-50 ℃ for 1-3 hours.
7. The method for preparing nano paillette silver powder as claimed in claim 1, wherein the step of centrifugal separation comprises standing the silver powder suspension, centrifuging at 3000-; then, adding the silver powder crude product into pure water, ethanol water solution and absolute ethanol in sequence, and respectively carrying out the following operations: centrifuging at 3000r/min (1000-.
8. The method for preparing nano spangle silver powder according to claim 1, wherein the drying temperature is 60-80 ℃, and the nano spangle silver powder is obtained by vacuum drying.
9. The nanometer paillette silver powder is characterized in that the nanometer paillette silver powder is irregular and flaky, has smooth surface, clear boundary between sheets, thickness of 40-70nm, sheet diameter less than or equal to 30 mu m and silver content more than 99.8 percent; the nano paillette silver powder can be partially sintered within the range of 200-; after being dried, the nano paillette silver powder is observed by naked eyes to be in a bright silver color.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001049309A (en) * | 1999-08-13 | 2001-02-20 | Dowa Mining Co Ltd | Silver powder, its production and production of flaky silver powder |
| CN1401452A (en) * | 2001-08-17 | 2003-03-12 | 中国科学院过程工程研究所 | Preparation of hexagonal plate silver powder by chemical reduction process |
| CN101342596A (en) * | 2008-07-21 | 2009-01-14 | 广东风华高新科技股份有限公司 | Process for preparing nm-class silver powder |
| CN101891238A (en) * | 2010-08-06 | 2010-11-24 | 浙江大学 | Method for hydrothermally synthesizing flaky erbium oxide nanostructure material |
| CN103506630A (en) * | 2012-06-29 | 2014-01-15 | 中国科学院理化技术研究所 | Method for preparing flaky silver powder with ultralow apparent density |
| CN104551009A (en) * | 2015-01-16 | 2015-04-29 | 吉林大学 | Preparation method of two-dimensional fractal silver nanoparticles in alcohol-water system |
| CN110303168A (en) * | 2019-08-06 | 2019-10-08 | 郴州市金贵银业股份有限公司 | A kind of preparation method of nano-silver powder |
| CN110340348A (en) * | 2019-08-05 | 2019-10-18 | 郴州市金贵银业股份有限公司 | A kind of nano-silver powder, preparation method, silver paste and application |
-
2019
- 2019-12-04 CN CN201911224686.1A patent/CN110919025B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001049309A (en) * | 1999-08-13 | 2001-02-20 | Dowa Mining Co Ltd | Silver powder, its production and production of flaky silver powder |
| CN1401452A (en) * | 2001-08-17 | 2003-03-12 | 中国科学院过程工程研究所 | Preparation of hexagonal plate silver powder by chemical reduction process |
| CN101342596A (en) * | 2008-07-21 | 2009-01-14 | 广东风华高新科技股份有限公司 | Process for preparing nm-class silver powder |
| CN101891238A (en) * | 2010-08-06 | 2010-11-24 | 浙江大学 | Method for hydrothermally synthesizing flaky erbium oxide nanostructure material |
| CN103506630A (en) * | 2012-06-29 | 2014-01-15 | 中国科学院理化技术研究所 | Method for preparing flaky silver powder with ultralow apparent density |
| CN104551009A (en) * | 2015-01-16 | 2015-04-29 | 吉林大学 | Preparation method of two-dimensional fractal silver nanoparticles in alcohol-water system |
| CN110340348A (en) * | 2019-08-05 | 2019-10-18 | 郴州市金贵银业股份有限公司 | A kind of nano-silver powder, preparation method, silver paste and application |
| CN110303168A (en) * | 2019-08-06 | 2019-10-08 | 郴州市金贵银业股份有限公司 | A kind of preparation method of nano-silver powder |
Non-Patent Citations (1)
| Title |
|---|
| 田晓霞等: "化学还原法制备不同形貌的纳米银粉", 《信息记录资料》 * |
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