CN112570728A - Flaky silver powder and preparation method and application thereof - Google Patents
Flaky silver powder and preparation method and application thereof Download PDFInfo
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- CN112570728A CN112570728A CN202011436036.6A CN202011436036A CN112570728A CN 112570728 A CN112570728 A CN 112570728A CN 202011436036 A CN202011436036 A CN 202011436036A CN 112570728 A CN112570728 A CN 112570728A
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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
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention relates to a flaky silver powder and a preparation method and application thereof, wherein the preparation method comprises the following steps: s1, dissolving a silver source in deionized water to prepare a silver ion-containing solution, dissolving a reducing agent in the deionized water to obtain a reducing agent solution, wherein the concentration range of silver ions in the silver ion-containing solution is 0.1-2 mol/L; s2, preparing a pH regulating solution, and adding the pH regulating solution into the silver ion-containing solution to regulate the pH value of the solution to 8-12; s3, adding the dispersing agent into the silver ion-containing solution and stirring uniformly; and S4, fully mixing and reducing the silver ion-containing solution and the reducing agent solution in the stirring process at the temperature of 20-60 ℃ to obtain silver particles, adding part of the reducing agent solution into part of the silver ion-containing solution in the mixing process, adding the rest of the reducing agent solution and the silver ion solution into the system simultaneously after fully reducing and stirring, continuously stirring and reducing until the reaction is finished, separating solid from liquid in the reaction solution, washing and drying to obtain the flaky silver powder. The method regulates and controls the particle size and the sheet size of the prepared silver powder, is easy to operate, and can meet different use requirements.
Description
Technical Field
The invention relates to conductive metal powder and a preparation method thereof, in particular to flaky silver powder and a preparation method and application thereof.
Background
The silver powder is used as the main component of the conductive silver paste and mainly plays a role of a functional phase in the silver paste. The parameters of the silver powder such as morphology, dispersibility, particle size and the like are directly related to the mechanical property, the electricity property and the printing property of the conductive paste, so that the conductivity of electronic components is influenced, and the quality of the silver powder determines whether the conductive paste can meet the requirement of the performance of electronic products.
At present, the silver powder used for the preparation of the conductive paste is mainly spherical silver powder and flake silver powder. Among them, the silver flakes are an important constituent of an electrode paste for surface mount components. The flaky silver powder has larger contact surface than the point contact of the spherical silver powder because the contact among the particles is surface contact or line contact, the resistance is relatively lower, and the conductivity is better; meanwhile, compared with silver powder with other shapes, the flaky silver powder with the same quality has larger coating area, and the use amount of the silver powder can be saved and the thickness of the coating can be reduced by adopting the flaky silver powder, so that the miniaturization of electronic components is facilitated. At present, in industrial production, a chemical reduction method is mainly used for preparing spherical silver powder, and then the spherical silver powder is pressed into a flaky silver powder by a mechanical ball milling method to obtain flaky silver powder, but the variable factors are more in the ball milling process, different batches are difficult to control, and impurities are easy to introduce in the ball milling process.
The invention patent of China with the application number of 201911250739.7 discloses a preparation method of flaky nano silver powder, which is characterized in that a dispersing agent is added into a reducing agent solution, and then the dispersing agent and a silver ammonia solution are mixed and heated to react to prepare the nano silver powder. In addition, the preparation method adds the mixed solution containing the reducing agent into the silver-ammonia solution in a dropwise manner, so that the whole preparation time is longer, and the power consumption cost of the whole production is higher. In addition, a Chinese patent with the application number of 201711060549.X discloses a method for preparing nanoscale flaky silver powder by a chemical method, but in the operation, a seed crystal needs to be prepared by silver nitrate alone, the operation is complicated, the subsequent cleaning difficulty is increased by adding three surfactants, the types of residual substances on the surface are increased, and the product use is easily influenced. Therefore, a new method for preparing flake silver powder is needed, which is more suitable for producing flake silver powder for mass application.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention provides the flaky silver powder and the preparation method and the application thereof, the silver powder is prepared by adopting a chemical reduction method, the product can be directly obtained in one step, the preparation process is simplified, the problems in the mechanical preparation can be avoided, the obtained silver powder is flaky in appearance, the reproducibility of the silver powder preparation is good, substances added in the preparation process are easy to clean and remove, and the flaky silver powder can be used as conductive paste to be used in the field of electronic functional materials correspondingly.
The preparation method of the flaky silver powder comprises the following steps:
s1, dissolving a silver source in deionized water to prepare a silver ion-containing solution, dissolving a reducing agent in the deionized water to obtain a reducing agent solution, wherein the concentration range of silver ions in the silver ion-containing solution is 0.1-2 mol/L;
s2, preparing a pH regulating solution, and adding the pH regulating solution into the silver ion-containing solution to regulate the pH value of the solution to 8-12;
s3, adding the dispersing agent into the silver ion-containing solution and stirring uniformly;
and S4, fully mixing and reducing the silver ion-containing solution and the reducing agent solution in the stirring process at the temperature of 20-60 ℃ to obtain silver particles, adding part of the reducing agent solution into part of the silver ion-containing solution in the mixing process, adding the rest of the reducing agent solution and the silver ion solution into the system simultaneously after fully reducing and stirring, continuously stirring and reducing until the reaction is finished, separating solid from liquid in the reaction solution, washing and drying to obtain the flaky silver powder.
Preferably, in step S1, the concentration of silver ions ranges from 0.1 mol/L to 0.5 mol/L.
Further, in step S1, the silver source is one or a mixture of silver nitrate and silver oxalate. Preferably silver nitrate is the silver source.
Further, in step S1, the reducing agent includes one of ascorbic acid, glucose, hydrazine hydrate or hydrogen peroxide, water is used as a solvent, and the reducing agent is added in an excess amount of 1-2 times as much as the silver ion.
Preferably, the reducing agent is ascorbic acid, and the addition amount thereof is 1.1 to 1.3 times.
Further, in step S2, the pH adjusting solution is an alkaline adjusting agent, and the alkaline adjusting agent is one or a mixture of ammonia water, sodium hydroxide and potassium hydroxide.
Preferably, the pH value in step S2 is 8-10, and the alkaline regulator is ammonia water.
Specifically, the pH adjustment comprises the specific steps of dropwise adding an alkaline regulator into the prepared silver ion-containing solution to adjust the pH value, and metering and determining the amount of the alkaline regulator and the adjustment end point by using a pH meter monitoring system.
Further, the dispersant in step S3 includes any one of citric acid, sodium citrate, polyvinylpyrrolidone, polymethacrylamide and ethyl cellulose, and the content of the dispersant is 1 wt% to 30 wt% of the silver source.
Specifically, the dispersant is in a powder form.
Preferably, the dispersant is one of polyvinylpyrrolidone or ethyl cellulose, and the content of the dispersant is 10 wt% to 20 wt% of the silver source.
Preferably, the dispersant is polyvinylpyrrolidone; after the reaction is finished and the solid-liquid separation is carried out on the reaction liquid, the reaction liquid is washed for 3-5 times by deionized water and then washed for 1 time by ethanol to remove surface impurities.
Further preferably, the dispersing agent is ethyl cellulose, and the ethyl cellulose is dissolved by an organic solvent and then added into the silver ion solution; after the reaction is finished, the solid-liquid separation of the reaction liquid is carried out, and the deionized water is used for washing for 1 time to remove surface impurities.
Specifically, the organic solvent is one of methanol or ethanol, preferably ethanol.
Further, in step S4, the ratio of the reducing agent solution to the silver ion-containing solution is 20% to 80% for the first time, after sufficient reduction stirring for a period of time, the remaining reducing agent solution and silver ion-containing solution are simultaneously added to the reacted system through a peristaltic pump to reduce and obtain silver particles, and the sample addition rate of the peristaltic pump is kept consistent.
Furthermore, the stirring manner is mechanical stirring, and the speed is 800-1200 r/min.
Preferably, the adding time is 1-2min, and the reaction temperature is controlled at 25-35 ℃.
Specifically, after solid-liquid separation of silver particles obtained after the reaction is finished, washing with deionized water and ethanol to remove surface impurities, and drying in an oven to obtain the micron-sized flaky silver powder.
More specifically, the solid-liquid separation mode is suction filtration, and the drying temperature in an oven is 75-85 ℃ for 2-3 h.
The flake silver powder is prepared by the method, the flake diameter distribution of the silver powder is 1.0-5.0 mu m, and the thickness of a flake layer is less than 200 nm.
The conductive paste is prepared by uniformly mixing 75-85% of silver powder, 3-7% of glass powder and 12-18% of organic carrier and then passing the mixture through a rolling mill, wherein the sheet resistance range of the conductive paste prepared from the silver powder is 6-10m omega/□.
Preferably, the conductive paste comprises 80% of silver powder, 5% of glass frit and 15% of organic vehicle.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with the prior art that a plurality of mechanical ball milling methods are used in industrial production, the method for preparing the flake silver powder by adopting the chemical reduction method simplifies the preparation process, has low requirements on experimental equipment, can regulate and control the particle size and the flake size of the prepared silver powder by adjusting relevant conditions such as concentration, dispersant content, reaction temperature and the like, is easy to operate, and can meet different use requirements.
2. According to the invention, a mode of multiple sample adding is adopted, a part of reducing agent solution is added into a part of silver ion solution for reduction reaction to prepare the crystal seed, and the rest solution is added into a reaction system, so that the preparation flow of the crystal seed is simplified, the growth of the silver powder can be better controlled by utilizing the principle of a crystal seed method, the particle size and the sheet size of the flaky silver powder are controlled, and the uniformity of the prepared silver powder is improved.
3. The method has the advantages that various substances added into the system are low in toxicity and pollution, can be easily removed after the reaction is finished, the process flow is simple, the reaction rate can be controlled by adjusting the pH value of the silver ion-containing solution, so that the pH value of the final system is determined, the production conditions are better determined, the silver powder can be ensured to generate a better sheet structure, experimental exploration is facilitated, the concentrations of silver nitrate and a reducing agent of the system at all times are similar in a symmetrical liquid adding mode, and the particles of the final product are more uniform, so that the method is suitable for large-scale industrial production.
4. The dispersant ethyl cellulose used in the reaction can be used as a thickener for preparing an organic carrier in the conductive paste, so that the subsequent cleaning is carried out for 1 time, the cleaning process is effectively reduced, the operation flow for preparing the silver powder is further simplified, and the subsequent use cannot be influenced by part of the residual dispersant.
5. The prepared silver powder has a good micron-scale sheet structure, and can be widely applied to the fields of conductive paste, photosensitive materials, electrode materials, decorative materials, silver alloy solder, composite materials, energy fields, silver-series antibacterial materials, silver catalysis industry and the like; particularly, the conductive paste can be further prepared and can be correspondingly used in the field of electronic functional materials as the conductive paste.
Drawings
FIG. 1 is a scanning electron micrograph of the silver flake obtained in example 1;
FIG. 2 is a scanning electron micrograph of the silver flake obtained in example 2;
FIG. 3 is a scanning electron micrograph of the silver flake obtained in example 3;
FIG. 4 is a scanning electron microscope picture of the silver powder obtained in comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
Adding 10g of silver nitrate into 250g of deionized water, fully stirring and dissolving, and adding 1g of polyvinylpyrrolidone into the silver nitrate solution; dissolving 6.5g of ascorbic acid in 250g of deionized water to prepare a reducing agent solution; adding an ammonia water solution into the silver nitrate solution to adjust the pH value to 10, and stirring to clarify the solution, wherein the concentration of silver ions in the silver ion-containing solution is 0.24mol/L, and the dispersing agent accounts for 10 wt% of a silver source; adding 20% ascorbic acid solution into 20% silver nitrate solution, stirring thoroughly for reduction, adding the rest silver nitrate solution and ascorbic acid solution into the reaction solution 20min later by using a peristaltic pump, and continuing stirring for reduction at a stirring speed of 1000r/min and a reaction temperature of 20 ℃.
And after the reaction is finished, carrying out solid-liquid separation on the reaction liquid, washing with deionized water for 3 times, washing with ethanol for 1 time, drying in an oven at 80 ℃ for 2 hours to obtain silver powder, wherein a scanning electron microscope picture is shown in figure 1.
Mixing the obtained silver powder with glass powder and an organic carrier according to a ratio of 80% of the silver powder, 5% of the glass powder and 15% of the organic carrier, uniformly stirring, passing through a three-roll mill to obtain conductive paste (silver paste), wherein the sheet resistance range is 6.8m omega/□, and sintering after silk-screen printing to obtain the conductive circuit.
Example 2
Dissolving 10g of silver nitrate into 250g of deionized water, and adding 1.5g of polyvinylpyrrolidone into the silver nitrate solution; dissolving 6.5g of ascorbic acid in 250g of deionized water to prepare a reducing agent solution; adding an ammonia water solution into the silver nitrate solution to adjust the pH value to 10, and stirring to clarify the solution, wherein the concentration of silver ions in the silver ion-containing solution is 0.24mol/L, and the dispersing agent accounts for 15 wt% of a silver source; adding 20% ascorbic acid solution into 20% silver nitrate solution, stirring thoroughly for reduction, adding the rest silver nitrate solution and ascorbic acid solution into the reaction solution 20min later by using a peristaltic pump, and continuing stirring for reduction at a stirring speed of 1000r/min and a reaction temperature of 25 ℃.
And after the reaction is finished, carrying out solid-liquid separation on the reaction liquid, washing with deionized water for 3 times, washing with ethanol for 1 time, drying in an oven at 80 ℃ for 2 hours to obtain silver powder, wherein a scanning electron microscope picture is shown in figure 2.
And mixing the obtained silver powder with glass powder and an organic carrier according to a ratio of 84% of the silver powder, 4% of the glass powder and 12% of the organic carrier, uniformly stirring, and then passing through a three-roll mill to obtain conductive paste (silver paste), wherein the sheet resistance range is 7.5m omega/□.
Example 3
Dissolving 10g of silver nitrate into 250g of deionized water, fully dissolving 1.5g of ethyl cellulose into 20ml of ethanol, adding the ethyl cellulose solution into the silver nitrate solution, and fully and uniformly mixing; dissolving 6.5g of ascorbic acid in 250g of deionized water to prepare a reducing agent solution; adding an ammonia water solution into the silver nitrate solution to adjust the pH value to 9, and stirring to clarify the solution, wherein the concentration of silver ions in the silver ion-containing solution is 0.24mol/L, and the dispersing agent accounts for 15 wt% of a silver source; adding 40% ascorbic acid solution into 40% silver nitrate solution, stirring thoroughly for reduction, adding the rest silver nitrate solution and ascorbic acid solution into the reaction solution 20min later by using a peristaltic pump, and continuing stirring for reduction at a stirring speed of 900r/min and a reaction temperature of 35 ℃.
And after the reaction is finished, carrying out solid-liquid separation on the reaction liquid, washing with deionized water for 1 time to remove surface impurities, drying in an oven at 80 ℃ for 2 hours to obtain silver powder, wherein a scanning electron microscope picture is shown in figure 3.
And mixing the obtained silver powder with glass powder and an organic carrier according to a ratio of 77% of the silver powder, 6% of the glass powder and 17% of the organic carrier, uniformly stirring, and then passing through a three-roll mill to obtain conductive paste (silver paste), wherein the sheet resistance range is 7.1m omega/□.
Example 4
Dissolving 35g of silver nitrate into 250g of deionized water, fully dissolving 4.5g of ethyl cellulose into 20ml of ethanol, adding the ethyl cellulose solution into the silver nitrate solution, and fully and uniformly mixing; dissolving 23g of glucose in 250g of deionized water to prepare a reducing agent solution; adding an ammonia water solution into the silver nitrate solution to adjust the pH value to 8, and stirring to clarify the solution, wherein the concentration of silver ions in the silver ion-containing solution is 0.83mol/L, and the dispersing agent accounts for 12.8 wt% of a silver source; adding 65% glucose solution into 65% silver nitrate solution, stirring thoroughly, reducing, adding the rest silver nitrate solution and ascorbic acid solution into the reaction solution with peristaltic pump after 25min, stirring continuously at a speed of 1100r/min, and controlling the reaction temperature at 20 deg.C.
And after the reaction is finished, carrying out solid-liquid separation on the reaction liquid, washing the reaction liquid with deionized water for 1 time to remove surface impurities, drying the reaction liquid in an oven at the temperature of 80 ℃ for 2 hours to obtain the silver powder, and washing the silver powder with the deionized water and then washing the silver powder with ethanol once.
And mixing the obtained silver powder with glass powder and an organic carrier according to a ratio of 78% of the silver powder, 6% of the glass powder and 16% of the organic carrier, uniformly stirring, and then passing through a three-roll mill to obtain conductive paste (silver paste), wherein the sheet resistance range is 7.9m omega/□.
Example 5
Dissolving 20g of silver oxalate in 250g of deionized water, and adding 4g of citric acid into the silver oxalate solution; dissolving 5g and 30% hydrogen peroxide in 250g deionized water to prepare a reducing agent solution; adding an ammonia water solution into the silver oxalate solution to adjust the pH value to 11, and stirring to clarify the solution, wherein the concentration of silver ions in the silver ion-containing solution is 0.53mol/L, and the dispersing agent is 20 wt% of a silver source; adding 20% hydrogen peroxide solution into 20% silver nitrate solution, stirring thoroughly for reduction, adding the rest silver nitrate solution and hydrogen peroxide solution into the reaction solution by using a peristaltic pump after 10min, and continuing stirring for reduction at a stirring speed of 800r/min and a reaction temperature of 55 ℃.
And after the reaction is finished, carrying out solid-liquid separation on the reaction liquid, washing with deionized water and ethanol to remove surface impurities, and drying in a 75 ℃ oven for 2.5 hours to obtain the silver powder.
And mixing the obtained silver powder with glass powder and an organic carrier according to a ratio of 83% of the silver powder, 4% of the glass powder and 13% of the organic carrier, uniformly stirring, and then passing through a three-roll mill to obtain conductive paste (silver paste), wherein the sheet resistance range is 9.2m omega/□.
Comparative description of experiments
Comparative example 1 below to control the silver powders prepared by different reaction acid-base ratios, the morphology of the silver powder prepared in comparative example 1 was compared with the silver powders prepared in examples 1 to 5.
Comparative example 1
Adding 10g of silver nitrate into 250g of deionized water, fully stirring and dissolving, and adding 1g of polyvinylpyrrolidone into the silver nitrate solution; dissolving 6.5g of ascorbic acid in 250g of deionized water to prepare a reducing agent solution; adding 20% ascorbic acid solution into 20% silver nitrate solution, stirring thoroughly, reducing, adding the rest silver nitrate solution and ascorbic acid solution into the reaction solution with peristaltic pump after 20min, and stirring continuously for reducing. And (3) after the reaction is finished, carrying out solid-liquid separation on the reaction liquid, washing with deionized water and ethanol to remove surface impurities, drying in an oven at 80 ℃ for 2 hours to obtain silver powder, wherein a scanning electron microscope picture is shown in figure 4, and the structure of the silver powder is similar to a sphere.
TABLE 1
According to the results, the silver powder prepared by the method has a micron-scale flaky structure, is good in uniformity and is suitable for industrial large-scale stable production.
Claims (10)
1. A preparation method of flaky silver powder is characterized by comprising the following steps:
s1, dissolving a silver source in deionized water to prepare a silver ion-containing solution, dissolving a reducing agent in the deionized water to obtain a reducing agent solution, wherein the concentration range of silver ions in the silver ion-containing solution is 0.1-2 mol/L;
s2, preparing a pH regulating solution, and adding the pH regulating solution into the silver ion-containing solution to regulate the pH value of the solution to 8-12;
s3, adding the dispersing agent into the silver ion-containing solution and stirring uniformly;
and S4, fully mixing and reducing the silver ion-containing solution and the reducing agent solution in the stirring process at the temperature of 20-60 ℃ to obtain silver particles, adding part of the reducing agent solution into part of the silver ion-containing solution in the mixing process, adding the rest of the reducing agent solution and the silver ion solution into the system simultaneously after fully reducing and stirring, continuously stirring and reducing until the reaction is finished, separating solid from liquid in the reaction solution, washing and drying to obtain the flaky silver powder.
2. The method for producing the plate-like silver powder according to claim 1, wherein in step S1, the silver source is one or a mixture of silver nitrate and silver oxalate.
3. The method for producing the plate-like silver powder according to claim 1 or 2, wherein the reducing agent comprises one of ascorbic acid, glucose, hydrazine hydrate or hydrogen peroxide, and water is used as a solvent in step S1, and the reducing agent is added in an excess amount of 1 to 2 times as much as silver ions.
4. The method for producing the plate-like silver powder according to claim 3, wherein in step S2, the pH adjusting liquid is an alkaline adjusting agent, and the alkaline adjusting agent is one or a mixture of ammonia water, sodium hydroxide and potassium hydroxide.
5. The method for producing the plate-like silver powder according to claim 4, wherein the dispersant in step S3 includes any one of citric acid, sodium citrate, polyvinylpyrrolidone, polymethacrylamide, and ethylcellulose, and the content of the dispersant is 1 to 30 wt% of the silver source.
6. The method for producing the plate-like silver powder according to claim 5, characterized in that the dispersant is polyvinylpyrrolidone; after the reaction is finished and the solid-liquid separation is carried out on the reaction liquid, the reaction liquid is washed for 3-5 times by deionized water and then washed for 1 time by ethanol to remove surface impurities, wherein the content of the dispersing agent is 10-20 wt% of the silver source.
7. The method for producing the silver flake according to claim 5, wherein the dispersant is ethyl cellulose, and the ethyl cellulose is dissolved in an organic solvent and then added to the silver ion solution; after the reaction is finished, the solid-liquid separation of the reaction liquid is carried out, and the deionized water is used for washing for 1 time to remove surface impurities.
8. The method for preparing silver flake according to claim 7, wherein in step S4, the ratio of the reducing agent solution and the silver ion-containing solution added for the first time is 20-80%, after fully reducing and stirring for a period of time, the remaining reducing agent solution and the silver ion-containing solution are simultaneously added to the reacted system by a peristaltic pump to reduce and obtain silver particles, the sample addition rate of the peristaltic pump is kept consistent, and the reaction temperature is controlled at 20-60 ℃.
9. Silver powder obtained based on a process for the preparation of silver powder in the form of flakes, characterized in that it has a distribution of plate diameters of 1.0-5.0 μm and a lamella thickness <200nm, obtainable according to the process of any one of claims 1-8.
10. An electroconductive paste, characterized in that the silver powder prepared by the method according to any one of claims 1 to 8 is prepared by uniformly mixing 75 to 85% of silver powder, 3 to 7% of glass frit and 12 to 18% of organic vehicle, and then passing the mixture through a rolling mill, wherein the sheet resistance ranges from 6 to 10m Ω/□.
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| CN113458410A (en) * | 2021-06-30 | 2021-10-01 | 东北大学 | With H2O2Method for synthesizing nano silver with various micro-morphologies as reducing agent |
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