CN117123794A - Micron silver particles with nanoscale rod-like structures on the surface and preparation method thereof - Google Patents
Micron silver particles with nanoscale rod-like structures on the surface and preparation method thereof Download PDFInfo
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- CN117123794A CN117123794A CN202311066657.3A CN202311066657A CN117123794A CN 117123794 A CN117123794 A CN 117123794A CN 202311066657 A CN202311066657 A CN 202311066657A CN 117123794 A CN117123794 A CN 117123794A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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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- 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
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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
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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
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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Abstract
The invention provides a micron silver particle with a nanoscale rod-shaped structure on the surface and a preparation method thereof, wherein the preparation method comprises the following steps: preparing a precursor solution, wherein the precursor solution contains a silver source and a coating agent; preparing a reducing solution, wherein the reducing solution contains a reducing agent; mixing the reduction solution and the precursor solution at 25-60 ℃ for oxidation-reduction reaction for 0.1-2.5 h, adding a self-assembly active agent for reaction for 1-2h, centrifuging, taking out precipitate, cleaning and drying to obtain micron silver particles with nanoscale rod-shaped structures on the surfaces; wherein the self-assembly active agent is at least one of sodium carbonate, sodium nitrate and sodium sulfate, and the mass ratio of silver ions to the self-assembly active agent is 5.0-10.0. By adopting the technical scheme of the invention, the micron silver particles with the nanoscale rod-shaped structures on the surfaces are obtained, and the particles are uniform and stable in size and shape and good in dispersibility.
Description
Technical Field
The invention belongs to the technical field of micro-nano metal materials, and particularly relates to a micron silver particle with a nanoscale rod-shaped structure on the surface and a preparation method thereof.
Background
The nano material has nano size effect and the like because the size is between 1 and 100nm, and the melting point of the nano material is obviously reduced and has special physicochemical properties. Among various nano metals, nano silver has been attracting attention due to its other special physicochemical properties of high heat conduction, high conductivity, antibacterial property, excellent catalytic activity, etc., and is widely used in various fields such as biomedical, catalytic, optical, electronic packaging, electromagnetic shielding, flexible materials, etc., wherein synthesis and preparation of nano silver particles have been one of the popular fields of research by vast material students. The existing common preparation methods of the nano silver particles mainly comprise a chemical method such as a liquid phase reduction method and the like, and a physical method such as a freezing ball milling method, a high-temperature ball milling method and the like. The surfaces of the nano silver particles obtained by the preparation methods all adopt organic coating layers to prevent the agglomeration phenomenon of the nano silver particles, and the spherical, triangular, cubic, tetrahedral, octahedral, decahedral, linear and rod-shaped nano silver particles can be prepared by the existing chemical method. However, due to the high surface energy of the nano silver particles, the agglomeration phenomenon is easy to occur frequently in spite of the existence of the coating agent, and the nano silver particles can lose the nano-size effect and lose the activity to influence the use. In contrast, micrometer metallic materials are generally prepared by physical methods, and generally have good dispersibility and uniform size due to steric hindrance caused by larger size of the micrometer metallic materials, but have larger size and poorer activity than nanometer materials.
Meanwhile, the control of the size uniformity of the nano silver particles and the mass production have a certain problem, and the micro silver particles can realize the mass production but lack the unique physical and chemical properties brought by the nano size effect. The advantages of the nano silver particles and the micro silver particles are combined, and the preparation process of the micro silver particles with the nano-sized structure on the surface is particularly important, wherein the preparation process is low in cost and simple in flow.
Disclosure of Invention
Aiming at the technical problems, the invention discloses a preparation method of micron silver particles with a nanoscale rod-shaped structure on the surface, the steric hindrance effect generated by the micron size of the obtained micron silver particles can effectively solve the problem of particle agglomeration, and the nanoscale rod-shaped structure on the surface of the particles can provide higher surface activity and higher specific surface area.
In this regard, the invention adopts the following technical scheme:
the preparation method of the micron silver particles with the nanoscale rod-shaped structures on the surfaces comprises the following steps:
step S1, preparing a precursor solution, wherein the precursor solution contains a silver source and a coating agent;
preparing a reducing solution, wherein the reducing solution contains a reducing agent;
step S2, mixing the reduction solution and the precursor solution at 25-60 ℃, carrying out oxidation-reduction reaction for 0.1-2.5 h, adding a self-assembly active agent for reaction for 1-2h, centrifuging, taking out sediment, cleaning and drying to obtain micron silver particles with nanoscale rod-shaped structures on the surfaces;
wherein the self-assembly active agent is at least one of sodium carbonate, sodium nitrate and sodium sulfate, and the mass ratio of silver ions in the precursor solution to the substances of the self-assembly active agent is 5.0-10.0.
As a further improvement of the present invention, step S1 further includes preparing a self-assembled active agent solution, and in step S2, the self-assembled active agent is added in the form of a self-assembled active agent solution, and the solvent of the self-assembled active agent solution is one or more of water, ethanol, ethylene glycol, diethylene glycol.
As a further improvement of the invention, in the step S2, the stirring rotation speed of the mixing is 250-1000 r/min.
As a further improvement of the invention, the mass ratio of silver ions to the substances of the coating agent in the precursor solution is 0.5-2.0.
As a further improvement of the present invention, the concentration of the silver ions in the precursor solution is 0.1 to 1.25mol/L, and in step S2, the precursor solution is added dropwise to the reduction solution at a rate of 0.15mL to 2 mL/S.
As a further improvement of the present invention, in step S2, the mass ratio of silver ions in the precursor solution to the reducing agent in the reducing solution is 0.1 to 1.
As a further improvement of the present invention, in step S1, the silver source is at least one of silver nitrate, silver acetylacetonate, silver bromate, silver bromide, silver chloride, silver citrate, silver fluoride, silver iodate, silver iodide, silver nitrite, silver oxalate, silver carbonate, silver nitrite, silver phosphate, silver chlorate, silver perchlorate, and silver tetrafluoroborate; the coating agent is at least one of citric acid, sodium citrate, polyvinylpyrrolidone, cetyltrimethylammonium bromide, sodium dodecyl benzene sulfonate, dodecyl mercaptan, polyethylene glycol and polyacrylic acid.
As a further improvement of the invention, the reducing agent is at least one of sodium borohydride, hydrazine hydrate, citric acid, formic acid, sodium citrate, disodium citrate, ferrous sulfate, ascorbic acid, sodium ascorbate, hydroxylamine, aniline, glucose, ethylene glycol, polyethylene glycol, glycerol, polyvinylpyrrolidone and sodium sulfite.
As a further improvement of the present invention, the solvent of the precursor solution is at least one of water, methanol, ethanol, ethylene glycol, propanol, isopropanol, butanol, isobutanol, pentanol, isopentanol, diethylene glycol, toluene, and xylene.
As a further improvement of the present invention, the solvent of the reducing solution is at least one of water, methanol, ethanol, ethylene glycol, propanol, isopropanol, butanol, isobutanol, pentanol, isopentanol, diethylene glycol, toluene, and xylene.
As a further improvement of the invention, in the step S2, the centrifugal cleaning is carried out for 4 times by adopting deionized water or absolute ethyl alcohol, the rotating speed is 2500-5000 r/min, and the drying is carried out for 10-12 hours at 45-55 ℃ under the condition that the vacuum degree is less than 0.01MPa after the cleaning is finished.
The invention also discloses a micron silver particle with a nanoscale rod-shaped structure on the surface, which is prepared by adopting the preparation method of the micron silver particle with the nanoscale rod-shaped structure on the surface.
Compared with the prior art, the invention has the beneficial effects that:
firstly, according to the technical scheme, a silver source and a coating agent are mixed to prepare a precursor solution, a certain amount of reducing solution is prepared, then the precursor solution and the reducing solution are mixed with each other to generate oxidation-reduction reaction, the added coating agent coats the specific surface of a silver seed crystal, so that silver which is reduced subsequently is deposited selectively, rod-shaped nano silver particles are formed, then according to the addition of a self-assembly active agent, the self-assembly active agent and the silver particles form a competitive relationship with each other, and gradually form good combination with the coating agent, so that organic coating on the surface of the silver particles loaded by the nano rod is gradually desorbed, and the exposed crystal faces and crystal faces exposed by other nano rod-shaped silver particles are mutually contacted and diffused to complete self-assembly, so that the micron silver particles with the surface of a nano rod-shaped structure are formed.
Secondly, the preparation process of the technical scheme is green and low in consumption, the prepared micron silver particles have unique rod-shaped nano structures on the surfaces, are uniform and stable in particle size and shape and good in dispersibility, can be produced in batches, and can be applied to the fields of electronic packaging, catalysis, antibiosis and the like.
Drawings
FIG. 1 is a field emission scanning electron microscope (SEM, ×50000) image of the micro silver particles obtained in example 1 of the present invention.
Fig. 2 is a field emission scanning electron microscope (SEM, ×5000) image of the micro silver particles obtained in example 1 of the present invention.
Fig. 3 is a field emission scanning electron microscope (SEM, ×50000) image of the internal structure of the micro silver particles in example 1 of the present invention.
Fig. 4 is an XRD pattern of the micro silver particles in example 1 of the present invention.
Fig. 5 is a field emission scanning electron microscope (SEM, ×20000) image of micro silver particles in example 6 of the present invention.
Fig. 6 is a field emission scanning electron microscope image of silver particles obtained in comparative example 3 of the present invention.
Detailed Description
Preferred embodiments of the present invention are described in further detail below.
The preparation method of the micron silver particles with the nanoscale rod-shaped structures on the surfaces comprises the following steps of:
step S1, preparing a precursor solution containing a silver source and a coating agent, a reducing solution containing a reducing agent and a solution containing a self-assembly active agent respectively;
step 2, mixing the precursor solution and the reducing solution, performing oxidation-reduction reaction at 25-60 ℃, adding self-assembled active agent solution after 0.1-2.5 h of reaction, and performing centrifugation, precipitation, cleaning and drying on the obtained solution to obtain micron silver particles with nanoscale rod-shaped structures on the surfaces;
wherein, during the oxidation-reduction reaction, the concentration of silver ions in the precursor solution is 0.1-1.25 mol/L, and the mass ratio of silver ions of the silver source to substances of the coating agent in the precursor solution is 0.5-2.0.
When the step S2 is carried out, the mass ratio of the silver ions of the silver source to the substances of the reducing agent in the reducing solution is 0.1-1; the mass ratio of silver ions to the self-assembled active agent in the precursor solution is 5.0-10.0. Further, the redox reaction is carried out under stirring, and the stirring speed is 250-1000 r/min.
Wherein, in the precursor solution, the silver source is one or more of silver nitrate, silver acetylacetonate, silver bromate, silver bromide, silver chloride, silver citrate, silver fluoride, silver iodate, silver iodide, silver nitrite, silver oxalate, silver carbonate, silver nitrite, silver phosphate, silver chlorate, silver perchlorate and silver tetrafluoroborate; the coating agent is one or more than two selected from citric acid, sodium citrate, polyvinylpyrrolidone, cetyltrimethylammonium bromide, sodium dodecyl benzene sulfonate, dodecyl mercaptan, polyethylene glycol and polyacrylic acid.
The solvent of the precursor solution and the solvent of the reducing solution are respectively and independently selected from one or more than two of water, methanol, ethanol, glycol, propanol, isopropanol, butanol, isobutanol, amyl alcohol, isoamyl alcohol, diethylene glycol, toluene and xylene.
In the reducing solution, the reducing agent is one or more than two selected from sodium borohydride, hydrazine hydrate, citric acid, formic acid, sodium citrate, disodium citrate, ferrous sulfate, ascorbic acid, sodium ascorbate, hydroxylamine, aniline, glucose, glycol, polyethylene glycol, glycerol, polyvinylpyrrolidone and sodium sulfite.
The self-assembly active agent is selected from one or more of sodium carbonate, sodium nitrate and sodium sulfate, and the solvent of the self-assembly active agent solution is selected from one or more of water, ethanol, glycol and diethylene glycol.
Preferably, mixing the precursor solution and the reducing agent solution with each other includes:
heating the precursor solution to 25-60 ℃, and then dropwise adding the reducing solution into the precursor solution; or heating the reducing solution to 25-60 ℃, and then dropwise adding the precursor solution into the reducing solution.
Preferably, the time of the oxidation-reduction reaction is 0.1-2.5 h, and after the oxidation-reduction reaction is finished, the self-assembly reaction is carried out for 1-2h after the self-assembly active agent solution is dripped.
Preferably, centrifuging the system after the self-assembly reaction is finished, taking out the precipitate, and washing and cleaning the system by deionized water or absolute ethyl alcohol, wherein the centrifugal cleaning condition is that the centrifugal cleaning is carried out for 4 times at a speed of 2500-5000 r/min for 4 minutes each time, and drying the system for 10-12 hours at a temperature of 50 ℃ under a vacuum degree of less than 0.01MPa after the cleaning is finished, so as to obtain the micro silver particles.
Example 1
3.4g of silver nitrate and 1.20g of polyvinylpyrrolidone are dispersed in 25ml of deionized water and stirred uniformly to form a precursor solution, then 3.04g of ferrous sulfate is dispersed in 25ml of deionized water and stirred uniformly to form a reducing solution, and then 0.40g of sodium sulfate is dispersed in 10ml of deionized water to form a self-assembly active agent solution. And (3) dropwise adding a reducing solution into the precursor solution at the stirring speed of 800r/min at room temperature at the speed of 1mL/s, dropwise adding a self-assembled active agent solution into a reaction system at the speed of 1mL/s after reacting for 10min, reacting for 30min again, centrifuging after the reaction is finished, taking out a precipitate after the reaction is finished, washing the precipitate with 3500r/min deionized water for 3 times, washing the precipitate with absolute ethyl alcohol once, and then drying the precipitate at 50 ℃ for 11h under the condition that the vacuum degree is less than 0.01MPa to obtain the micron silver particles with the nanoscale rod-shaped structure.
Taking the obtained micron silver particles with the nanoscale rod-shaped structures on the surfaces, observing the morphology of the particles by using a field emission Scanning Electron Microscope (SEM), and carrying out phase-spectrum analysis on the particles by using an X-ray diffractometer (XRD). The results are shown in fig. 1, 2, 3 and 4, respectively. As can be seen from fig. 1, a plurality of nano rod-like structures exist on the surface of the micro silver particles, and the nano rod-like structures are uniformly distributed on the surface of the micro silver particles; as can be seen from FIG. 2, the micron silver particles have good dispersibility, no obvious agglomeration phenomenon, uniform particle size and uniform shape. As can be seen from fig. 3, the whole silver microparticles are self-assembled by the nano silver rods, and the interior of the silver microparticles is a nano silver rod structure. The characteristic peaks of elemental metallic silver can be seen from fig. 4, where there are no characteristic peaks of silver oxide or second phase species.
Example 2
6.8g of silver nitrate and 6.88g of sodium citrate are dispersed in 75ml of deionized water and stirred uniformly to form a precursor solution, then 8.10g of ferrous sulfate is dispersed in 50ml of deionized water and stirred uniformly to form a reducing solution, and then 0.35g of sodium nitrate is dispersed in 15ml of deionized water to form a self-assembly active agent solution. And (3) dropwise adding a reducing solution into the precursor solution at the stirring speed of 600r/min at room temperature, reacting for 20min, dropwise adding a self-assembled active agent solution into a reaction system at the stirring speed of 0.5mL/s, reacting for 20min, washing with 3500r/min deionized water for 3 times after the reaction is finished, washing with absolute ethyl alcohol once, and then drying the precipitate at the temperature of 50 ℃ for 11h under the condition that the vacuum degree is less than 0.01MPa to obtain the nano-rod-like silver particles.
The SEM image, XRD image and internal structure of the prepared micron silver particles are similar to those of the example 1, which shows that the micron silver particles are metallic silver simple substance, have no other impurities, have no agglomeration phenomenon, are well dispersed and have uniform particle size.
Example 3
3.4g of silver nitrate and 3.44g of sodium citrate are dispersed in 50ml of deionized water and stirred uniformly to form a precursor solution, then 16.48g of ascorbic acid is dispersed in 50ml of deionized water and stirred uniformly to form a reducing solution, and then 0.32g of sodium nitrate is dispersed in 10ml of deionized water to form a self-assembled active agent solution. And (3) dropwise adding a reducing solution into the precursor solution at the speed of 0.5mL/s when the stirring speed is 400r/min at the water bath temperature of 50 ℃, dropwise adding a self-assembled active agent solution into a reaction system at the speed of 0.5mL/s after reacting for 30min, reacting for 1.5h, washing with deionized water at 4000r/min for 3 times after the reaction is finished, washing with absolute ethyl alcohol once, and then drying the precipitate at the temperature of 50 ℃ for 10h under the condition that the vacuum degree is less than 0.01MPa to obtain the nano-level rod-shaped silver particles.
The SEM image, XRD image and internal structure of the prepared micron silver particles are similar to those of the example 1, which shows that the micron silver particles are metallic silver simple substance, have no other impurities, have no agglomeration phenomenon, are well dispersed and have uniform particle size.
Example 4
1.7g of silver nitrate and 1.15g of polyvinylpyrrolidone are dispersed in 25ml of ethylene glycol and stirred uniformly to obtain a precursor solution, then 2.0g of ascorbic acid is dispersed in 25ml of ethylene glycol and stirred uniformly to obtain a reducing solution, and then 0.11g of sodium nitrate is dispersed in 5ml of ethylene glycol to obtain a self-assembled active agent solution. And (3) dropwise adding a reducing solution into the precursor solution at the speed of 0.5mL/s when the stirring speed is 400r/min at the temperature of 60 ℃ in a water bath, dropwise adding a self-assembled active agent solution into a reaction system at the speed of 0.5mL/s after 0.5h of reaction, reacting for 1.5h, washing 3500r/min deionized water for 3 times after the reaction is finished, washing the washed product once by using absolute ethyl alcohol, and then drying the precipitate for 10h at 50 ℃ under the condition that the vacuum degree is less than 0.01MPa to obtain the nano-level rod-shaped silver particles.
The SEM image, XRD image and internal structure of the prepared micron silver particles are similar to those of the example 1, which shows that the micron silver particles are metallic silver simple substance, have no other impurities, have no agglomeration phenomenon, are well dispersed and have uniform particle size.
Example 5
2.55g of silver nitrate and 2.3g of citric acid are dispersed in 40ml of diethylene glycol and stirred uniformly to form a precursor solution, then 2.88g of ascorbic acid is dispersed in 40ml of diethylene glycol and stirred uniformly to form a reducing solution, and then 0.22g of sodium carbonate is dispersed in 5ml of diethylene glycol to form a self-assembled active agent solution. And (3) dropwise adding a reducing solution into the precursor solution at the speed of 0.5mL/s when the stirring speed is 400r/min at the temperature of 60 ℃ in a water bath, dropwise adding a self-assembled active agent solution into a reaction system at the speed of 0.5mL/s after reacting for 30min, reacting for 1.5h, washing 3500r/min deionized water for 3 times after the reaction is finished, washing the washed product with absolute ethyl alcohol once, and then drying the precipitate at the temperature of 50 ℃ for 10h under the condition that the vacuum degree is less than 0.01MPa to obtain the micron silver particles with the nanoscale rod-shaped structure.
The SEM image, XRD image and internal structure of the prepared micron silver particles are similar to those of the example 1, which shows that the micron silver particles are metallic silver simple substance, have no other impurities, have no agglomeration phenomenon, are well dispersed and have uniform particle size.
Comparative example 1
This comparative example 1 was different from example 1 in that the mass of sodium sulfate added in example 1 was changed to 0.57g, and the other conditions were exactly the same as in example 1.
The morphology of the silver particles obtained is shown in fig. 5, and it can be seen that for this example, due to the excessive addition of the self-assembled active agent, the assembly unit further assembles particles to form a sheet structure formed by assembling a plurality of particles after the assembly of the micro silver particles occurs.
Comparative example 2
This comparative example 2 is different from example 1 in that the mass of sodium sulfate added in example 1 was changed to 0.25g.
No particles similar to those of fig. 1 were obtained after preparation, and a large number of rod-like, spherical particles were obtained by observation, i.e. there was no way to spontaneously assemble together due to the small addition of minimal assembled units of self-assembling active agents.
As can be seen from the above examples and comparative examples, the micron silver particles with nanoscale rod-shaped structures on the surfaces, prepared by the method, use lower-cost raw materials as reactants, have low-consumption and environment-friendly reaction conditions, and have simple preparation flow. Meanwhile, the prepared micron silver particles have good dispersibility, the surfaces of the micron silver particles have consistent nanoscale rod-shaped structures, and the micron silver particles can be produced in batches and applied to the fields of electronic packaging materials, catalysis and the like.
Comparative example 3
The present comparative example differs from example 1 in that no self-assembling active agent was added.
After the preparation, no particles similar to those in fig. 1 were obtained, and particles similar to those in comparative example 2 were obtained, that is, no self-assembly active agent was added, and the smallest units of the silver particles at the initial stage of the reaction could not be self-assembled, and the prepared silver particles were as shown in fig. 6.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (10)
1. A preparation method of micron silver particles with nanoscale rod-shaped structures on surfaces is characterized by comprising the following steps of: the method comprises the following steps:
step S1, preparing a precursor solution, wherein the precursor solution contains a silver source and a coating agent;
preparing a reducing solution, wherein the reducing solution contains a reducing agent;
step S2, mixing the reduction solution and the precursor solution at 25-60 ℃, carrying out oxidation-reduction reaction for 0.1-2.5 h, adding a self-assembly active agent for reaction for 1-2h, centrifuging, taking out sediment, cleaning and drying to obtain micron silver particles with nanoscale rod-shaped structures on the surfaces;
wherein the self-assembly active agent is at least one of sodium carbonate, sodium nitrate and sodium sulfate, and the mass ratio of silver ions in the precursor solution to the substances of the self-assembly active agent is 5.0-10.0.
2. The method for preparing the micro silver particles with the nano rod-like structure on the surface according to claim 1, wherein the method comprises the following steps:
the step S1 further comprises preparing a self-assembly active agent solution, and in the step S2, the self-assembly active agent is added in the form of the self-assembly active agent solution, and the solvent of the self-assembly active agent solution is one or more than two of water, ethanol, glycol and diethylene glycol.
3. The method for preparing the micro silver particles with the nano rod-like structure on the surface according to claim 1, wherein the method comprises the following steps: in the precursor solution, the mass ratio of silver ions to the substances of the coating agent is 0.5-2.0.
4. A method for producing micro silver particles having a nano-scale rod-like structure on the surface according to claim 3, characterized in that: in the precursor solution, the concentration of silver ions is 0.1-1.25 mol/L, and in the step S2, the precursor solution is dripped into the reduction solution at a speed of 0.15-2 mL/S.
5. The method for preparing the micro silver particles with the nano rod-like structure on the surface according to claim 4, wherein the method comprises the following steps: in the step S2, the mass ratio of silver ions in the precursor solution to the reducing agent in the reducing solution is 0.1-1.
6. The method for preparing the micro silver particles with the nano rod-like structure on the surface according to claim 1, wherein the method comprises the following steps: in the step S1, the silver source is at least one of silver nitrate, silver acetylacetonate, silver bromate, silver bromide, silver chloride, silver citrate, silver fluoride, silver iodate, silver iodide, silver nitrite, silver oxalate, silver carbonate, silver nitrite, silver phosphate, silver chlorate, silver perchlorate and silver tetrafluoroborate; the coating agent is at least one of citric acid, sodium citrate, polyvinylpyrrolidone, cetyltrimethylammonium bromide, sodium dodecyl benzene sulfonate, dodecyl mercaptan, polyethylene glycol and polyacrylic acid.
7. The method for preparing the micro silver particles with the nano rod-like structure on the surface according to claim 1, wherein the method comprises the following steps: the reducing agent is at least one of sodium borohydride, hydrazine hydrate, citric acid, formic acid, sodium citrate, disodium citrate, ferrous sulfate, ascorbic acid, sodium ascorbate, hydroxylamine, aniline, glucose, glycol, polyethylene glycol, glycerol, polyvinylpyrrolidone and sodium sulfite.
8. The method for preparing the micro silver particles with the nano rod-like structure on the surface according to claim 1, wherein the method comprises the following steps: the solvent of the precursor solution is at least one of water, methanol, ethanol, glycol, propanol, isopropanol, butanol, isobutanol, amyl alcohol, isoamyl alcohol, diethylene glycol, toluene and xylene;
the solvent of the reducing solution is at least one of water, methanol, ethanol, glycol, propanol, isopropanol, butanol, isobutanol, amyl alcohol, isoamyl alcohol, diethylene glycol, toluene and xylene.
9. The method for preparing the micro silver particles with the nano rod-like structure on the surface according to claim 1, wherein the method comprises the following steps: in the step S2, centrifugal cleaning is carried out for 4 times by adopting deionized water or absolute ethyl alcohol, the rotating speed is 2500-5000 r/min, and the cleaning is finished and then the cleaning is dried for 10-12 hours at 45-55 ℃ under the condition that the vacuum degree is less than 0.01 MPa.
10. A micron silver particle with a nanoscale rod-shaped structure on the surface, which is characterized in that: which is prepared by the preparation method of the micron silver particles with the nanoscale rod-shaped structures on the surfaces according to any one of claims 1 to 9.
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| CN117123793A (en) * | 2023-08-23 | 2023-11-28 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Mesoscopically structured micron silver, low-temperature sinterable solder paste and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117123793A (en) * | 2023-08-23 | 2023-11-28 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Mesoscopically structured micron silver, low-temperature sinterable solder paste and preparation method and application thereof |
| CN117123793B (en) * | 2023-08-23 | 2026-01-23 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Micro-silver with mesoscopic structure, soldering paste capable of being sintered at low temperature, and preparation method and application thereof |
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