CN111168083A - Preparation method of nano silver powder - Google Patents
Preparation method of nano silver powder Download PDFInfo
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- CN111168083A CN111168083A CN202010113341.5A CN202010113341A CN111168083A CN 111168083 A CN111168083 A CN 111168083A CN 202010113341 A CN202010113341 A CN 202010113341A CN 111168083 A CN111168083 A CN 111168083A
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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
- 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
Abstract
The invention discloses a preparation method of nano silver powder, which comprises the following steps: dissolving a silver source and a protective agent in polyhydric alcohol to prepare silver-containing solution; mixing an alkaline solution with a silver-containing solution, and carrying out hydrothermal reaction at a reaction temperature of 120-200 ℃; and collecting and separating the reaction product to obtain the nano silver powder, wherein the particle size of nano silver particles in the nano silver powder is 50-600 nm. According to the preparation method, the silver source and the polyhydric alcohol are used as raw materials, the nano silver powder is obtained through one-step reaction by a hydrothermal method, the reaction system of the preparation method is simple, no additional reducing agent is added, and the particle size of the nano silver can be controlled by controlling the hydrothermal condition.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a preparation method of nano silver powder.
Background
"nanometer" is a unit of length, and it is considered in the research field of nanotechnology that the size of a nanomaterial should be between 1nm and 100 nm. The unique microstructure of the nano material enables the nano material to have small size effect, surface effect, quantum size effect and macroscopic quantum tunneling effect, and the unique properties enable the nano material to have wide application in thermal, optical, electrical, magnetic and catalytic science. As a novel material, the nano material has a great number of applications in various industries and a plurality of fields closely related to people, and is widely applied to the fields of catalysis science, electronic information science, photographic technology, rapid information storage and the like. Therefore, the research of the nano material and the related application thereof in various fields, especially the synthesis and preparation of the nano material have become one of the research fields of the broad material researchers.
The nano metal material has become one of the hot spots in the research field of nano materials, wherein the nano silver wires and the nano silver particles have good physicochemical properties, have very high and super performances in the fields of information technology, antibacterial sterilization, catalytic science and the like, and have abundant application values which are paid attention to by a plurality of material science workers. The material has various applications in catalytic materials, optical materials, antibacterial materials, coating materials and the like.
Chinese patent CN 106964785a discloses a method for preparing nano silver particles, which comprises dissolving silver nitrate in a polyol solution, reacting at a certain temperature to synthesize silver particles with nano particle size, wherein the method has the advantages of low cost and high yield, but the particle size of the particles is larger, and the result is unstable.
Chinese patent CN 106623971a discloses a method for synthesizing stable silver nanoparticles, which adopts a mixed solution of a reducing agent and silver nitrate to synthesize stable silver nanoparticles, and includes two steps of mixing a silver source and an organic amine solution to obtain a mixed solution and synthesizing the silver nanoparticles, wherein silver nitrate is used as the silver source, hydrazine hydrate or sodium borohydride is used as the reducing agent, and organic amine is used as a protective agent.
The preparation process of the nano silver powder with controllable particle size has a few difficulties. Although other methods such as vapor deposition and vapor reduction can produce high-purity silver nanoparticles with few impurities, these methods require expensive experimental equipment and harsh experimental conditions. How to solve the technical problems in the prior art and provide a simpler preparation process of the nano silver powder with controllable particle size is very important.
Disclosure of Invention
In order to solve the problems that the preparation method of the nano silver powder in the prior art cannot combine the advantages of simple preparation process, stable reaction and controllable particle size of the product, the invention provides the preparation method of the nano silver powder, the preparation method has one-step reaction, the reaction system is simple, no additional reducing agent is added, and the particle size of the nano silver particles is controllable.
In order to achieve the above object, the present invention provides a method for preparing nano silver powder, comprising the steps of:
dissolving a silver source and a protective agent in polyhydric alcohol to prepare silver-containing solution;
mixing an alkaline solution with a silver-containing solution, and carrying out hydrothermal reaction at a reaction temperature of 120-200 ℃;
and collecting and separating the reaction product to obtain the nano silver powder, wherein the particle size of nano silver particles in the nano silver powder is 50-600 nm.
Preferably, the silver source is silver nitrate, silver trifluoroacetate, silver carbonate or silver acetate.
Preferably, the protective agent is at least one of sodium dodecylbenzene sulfonate, polyvinylpyrrolidone, polyvinyl alcohol, oleic acid, polyethylene glycol, n-dodecyl mercaptan, polyacrylic acid, and lauric acid.
Preferably, the polyhydric alcohol is at least one of ethylene glycol, 1, 2-propylene glycol, glycerol and pentaerythritol; the alkaline solution is sodium hydroxide solution, potassium hydroxide solution, sodium bicarbonate solution, sodium carbonate solution or ammonia water.
Preferably, the mass ratio of the silver source to the protective agent ranges from 1: (0.25 to 4); the mass ratio of the polyhydric alcohol to the silver source is in the range of 1: (0.01-0.1).
Preferably, the concentration range of the alkaline solution is 0.05-2 mol/L.
Preferably, the reaction time of the hydrothermal reaction is 1-12 h.
Preferably, the method of separating the reaction product comprises at least one of filtration, sedimentation, evaporation or centrifugation.
Preferably, the nano silver powder is washed and dried; the washing method comprises the steps of repeatedly washing the nano silver powder for 3-5 times by adopting absolute ethyl alcohol and/or deionized water; the drying method includes at least one of vacuum drying, natural drying, heat drying and forced air drying.
Further preferably, the temperature of the vacuum drying is 20-50 ℃.
According to the preparation method of the nano silver powder, the polyalcohol is used as a solvent and a reducing agent, silver ions in a silver source are reduced into simple substance nano silver under the hydrothermal condition, and the reaction conditions are regulated to obtain nano silver particles with different particle sizes.
Drawings
The above and other aspects, features and advantages of embodiments of the present invention will become more apparent from the following description taken in conjunction with the accompanying drawings, in which:
FIG. 1 is an XRD pattern of silver nanopowder in example 1 of the present invention;
FIG. 2 is an SEM photograph of silver nanoparticles in example 1 of the present invention;
FIG. 3 is an SEM photograph of silver nanoparticles in example 2 of the present invention;
FIG. 4 is an SEM photograph of silver nanoparticles in example 3 of the present invention;
FIG. 5 is an SEM photograph of silver nanoparticles in example 4 of the present invention;
FIG. 6 is an SEM photograph of silver nanoparticles in example 5 of the present invention.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail. This invention may, however, be embodied in many different forms and should not be construed as limited to the specific embodiments set forth herein. Rather, these embodiments are provided to explain the principles of the invention and its practical application to thereby enable others skilled in the art to understand the invention for various embodiments and with various modifications as are suited to the particular use contemplated.
The invention provides a preparation method of nano silver powder based on the problems that a preparation method of nano silver powder in the prior art cannot combine the advantages of simple preparation process, stable reaction and controllable particle size of a product.
The invention provides a preparation method of nano silver powder, which comprises the following steps:
step A: the silver source and the protective agent are dissolved in the polyhydric alcohol to prepare a silver-containing solution.
The silver source is used for providing silver ions, and can be silver nitrate, silver trifluoroacetate, silver carbonate or silver acetate and the like. Other silver compounds are slightly soluble in polyols and have little solubility, so silver nitrate is further preferred as the silver source.
The protective agent has the functions of: steric hindrance is generated to prevent the agglomeration and further growth of the nano silver particles. Preferably, the protective agent is at least one of sodium dodecylbenzene sulfonate, polyvinylpyrrolidone, polyvinyl alcohol, oleic acid, polyethylene glycol, n-dodecyl mercaptan, polyacrylic acid, and lauric acid, preferably a combination of sodium dodecylbenzene sulfonate and polyvinylpyrrolidone, a combination of polyvinyl alcohol and polyethylene glycol, and a combination of lauric acid and oleic acid.
The mass ratio of the silver source to the protective agent is preferably in the range of 1: (0.25-4). Such as 1:0.25, 1:0.5, 1:1, 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5 or 1:4, but not limited to the recited values, and other values not recited within the range of values are equally applicable, preferably 1:1. When the dosage of the protective agent is too high, on one hand, high residual rate is easily caused, and on the other hand, high cost is caused; when the amount of the protective agent is too small, it is difficult to achieve the desired effect of preventing agglomeration of product particles.
Since the actual production scale in the industry is not a fixed amount, the present invention does not specifically limit the mass value and the mass unit of each substance. For example, the mass range of silver nitrate adopted in the embodiment of the invention is 1-10 g, such as 1g, 2g, 3g, 4g, 5g, 6g, 7g, 8g, 9g or 10g, and the like, and more preferably 3 g; the mass range of the protective agent is 2-10 g, such as 2g, 3g, 4g, 5g, 6g, 7g, 9g or 10g, and the like, and the preferred mass range is 3 g.
The polyalcohol is used as a solvent and a reducing agent, has mild reducing capability, has great relation with temperature, and can well control the formation speed and the growth speed of nano-silver crystal nuclei by utilizing the different reducing capabilities of the polyalcohol at different temperatures so as to obtain nano-silver particles with different sizes, uniform appearance and good dispersibility. Preferably, the polyol is at least one of ethylene glycol, 1, 2-propylene glycol, glycerol and pentaerythritol. Typical combinations are, but not limited to, combinations of ethylene glycol and 1, 2-propylene glycol, combinations of 1, 2-propylene glycol and glycerol, combinations of glycerol and pentaerythritol, combinations of pentaerythritol and ethylene glycol or combinations of ethylene glycol, glycerol and pentaerythritol, and the like, preferably ethylene glycol or glycerol. It is further preferred that the mass ratio of the polyol to the silver source is in the range of 1: (0.01 to 0.1), and any other values not listed in the above numerical range are applicable.
The silver source and the protective agent are dissolved under stirring, and the stirring speed is 100-500 r/min. Such as 100r/min, 200r/min, 300r/min, 400r/min, or 500r/min, but not limited to the recited values, and other values not recited within the numerical range are equally applicable.
And B: mixing the alkaline solution with the silver-containing solution, and carrying out hydrothermal reaction at the reaction temperature of 120-200 ℃.
The alkaline solution is sodium hydroxide solution, potassium hydroxide solution, sodium bicarbonate solution, sodium carbonate solution or ammonia water. The alkaline solution can be prepared by dissolving soluble alkali in deionized water, and the specific selectable soluble alkali comprises sodium hydroxide, potassium hydroxide and the like; or an alkaline solution formed by dissolving a salt in water, such as sodium carbonate or sodium bicarbonate. Preferably, the concentration range of the alkaline solution is 0.05-2 mol/L.
The reaction temperature of the hydrothermal reaction is in the range of 120 to 200 ℃, for example, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, 180 ℃ or 200 ℃, but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
The reaction time of the hydrothermal reaction is preferably in the range of 1 to 12 hours, such as 1 hour, 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, 11 hours, or 12 hours, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
And C: and collecting and separating the reaction product to obtain the nano silver powder, wherein the particle size of nano silver particles in the nano silver powder is 50-600 nm.
The separation method of the reaction product includes at least one of filtration, sedimentation, evaporation or centrifugation, preferably centrifugation. Typical but non-limiting combinations are: combinations of filtration and settling, combinations of settling and evaporation, combinations of evaporation and centrifugation, combinations of centrifugation and filtration or combinations of evaporation, centrifugation and filtration, and the like.
Preferably, the nano silver powder is washed and dried.
The washing method comprises the step of repeatedly washing the nano silver powder for 3-5 times by adopting absolute ethyl alcohol and/or deionized water, and further preferably washing by matching with ultrasonic dispersion.
The drying method includes at least one of vacuum drying, natural drying, heat drying and forced air drying. Further preferably, the vacuum drying is carried out at the temperature of 20-50 ℃. The drying time is 12h to 24h, for example 12h, 15h, 18h, 21h or 24h, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
The particle size of the nano silver particles is in the range of 50nm to 600nm, and for example, 50nm, 100nm, 200nm, 300nm, 400nm, 500nm, 600nm and the like exist, but not limited to the enumerated values, and other unrecited values also exist in the numerical range. Of course, if there is a strict requirement for the particle size of the nano silver in the subsequent application scenario, the obtained nano silver powder may be further subjected to particle size screening according to the requirement.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the preparation method of the nano-silver particles simplifies the types of reactants, so that the reaction is easier to control, and the raw material and process cost is effectively reduced;
(2) the raw materials used in the invention are basically nontoxic, pollution-free and environment-friendly, wherein the polyhydric alcohol is used as a solvent and a reducing agent, so that the reaction steps are simplified;
(3) the invention can obtain the nano silver particles with controllable size by reacting under a certain temperature condition, has good reaction stability, and is easy to control and operate;
(4) the reaction device of the hydrothermal reaction is simple, and has good repeatability under proper reaction conditions.
The method for preparing the above-mentioned silver nanoparticles according to the present invention will be described below with reference to specific examples, and it will be understood by those skilled in the art that the following examples are only specific examples of the method for preparing the above-mentioned silver nanoparticles according to the present invention, and are not intended to limit the entirety thereof.
Example 1
(1) 2g of silver nitrate and 2g of polyvinylpyrrolidone are weighed and placed in a beaker, 100g of 1, 2-propylene glycol is added, and the mixture is stirred at room temperature at a speed of 100r/min until all solid particles are dissolved, thereby preparing a silver ion-containing solution.
(2) At the same time, 0.2g of sodium hydroxide was weighed, added to 5g of deionized water, and stirred at room temperature until completely dissolved to prepare an alkaline solution.
(3) Mixing the silver ion-containing solution and the alkaline solution, transferring the mixed solution into a 250mL hydrothermal reaction kettle, placing the hydrothermal reaction kettle in a drying oven at 120 ℃ for constant-temperature reaction for 12 hours, and naturally cooling to room temperature. And centrifuging, collecting, washing and drying the reaction product to obtain the nano silver powder.
The nano silver powder obtained in example 1 was subjected to X-ray diffraction (abbreviated as XRD) study, and the obtained spectrum is shown in fig. 1, and it can be seen that the nano silver particles obtained in example 1 have higher purity compared with the standard silver card.
Scanning analysis is carried out on the silver nanoparticles by using a Scanning Electron Microscope (SEM), and an obtained electron microscope image is shown in FIG. 2. As can be seen from fig. 2, the nano silver particles in the nano silver powder obtained in the present embodiment are in a quasi-spherical structure, and have the characteristics of uniform particle size, good result repeatability, and stable morphology, and the particle size range is 50-80 nm.
Example 2
(1) 4g of silver nitrate and 2g of sodium dodecyl benzene sulfonate are weighed and placed in a beaker, 100g of ethylene glycol is added, and the mixture is stirred at room temperature at a speed of 150r/min until all solid particles are dissolved, so that the silver ion-containing solution is prepared.
(2) At the same time, 0.3g of sodium hydroxide was weighed, added to 6g of deionized water, and stirred at room temperature until completely dissolved to prepare an alkaline solution.
(3) Mixing the silver ion-containing solution and the alkaline solution, transferring the mixed solution into a 250mL hydrothermal reaction kettle, placing the hydrothermal reaction kettle in a drying oven at 130 ℃ for constant-temperature reaction for 6h, and naturally cooling to room temperature. And centrifuging, collecting, washing and drying the reaction product to obtain the nano silver powder.
Scanning analysis is carried out on the nano silver powder by adopting a scanning electron microscope, and an obtained electron microscope image is shown in figure 3. As can be seen from fig. 3, the particle size of the nano silver particles in the nano silver powder obtained in this embodiment is in the range of 60nm to 110nm, and the nano silver powder has a spheroidal shape and a small amount of short rod-like structures.
Example 3
(1) Weighing 4g of silver nitrate and 4g of polyacrylic acid, placing the silver nitrate and the polyacrylic acid in a beaker, adding 100g of glycerol, and stirring at the room temperature at the speed of 400r/min until all solid particles are dissolved to prepare the silver ion-containing solution.
(2) At the same time, 0.4g of sodium hydroxide was weighed, added to 8g of deionized water, and stirred at room temperature until completely dissolved to prepare an alkaline solution.
(3) Mixing the silver ion-containing solution and the alkaline solution, transferring the mixed solution into a 250mL hydrothermal reaction kettle, reacting for 2h in a drying oven at the constant temperature of 160 ℃, and naturally cooling to room temperature. And centrifuging, collecting, washing and drying the reaction product to obtain the nano silver powder.
Scanning analysis is carried out on the nano silver powder by adopting a scanning electron microscope, and an obtained electron microscope image is shown in figure 4. As can be seen from fig. 4, the nano silver particles in the nano silver powder obtained in this example have a particle size range of 180nm to 250nm, and have the characteristics of narrow distribution and good crystallinity. As can be seen from the comparison of the nano silver particles in example 2, the aggregation of the particles can be significantly improved by increasing the amount of the protective agent.
Example 4
(1) 3g of silver nitrate and 1.5g of polyvinyl alcohol were weighed and placed in a beaker, 50g of glycerol was added, and the mixture was stirred at room temperature at a speed of 200r/min until the solid particles were completely dissolved, to prepare a silver ion-containing solution.
(2) At the same time, 0.1g of sodium hydroxide was weighed, added to 3g of deionized water, and stirred at room temperature until completely dissolved to prepare an alkaline solution.
(3) Mixing the silver ion-containing solution and the alkaline solution, transferring the mixed solution into a 100mL hydrothermal reaction kettle, placing the hydrothermal reaction kettle in an oven at 180 ℃ for constant-temperature reaction for 1h, and naturally cooling to room temperature. And centrifuging, collecting, washing and drying the reaction product to obtain the nano silver powder.
Scanning analysis is carried out on the nano silver powder by adopting a scanning electron microscope, and an obtained electron microscope image is shown in figure 5. As can be seen from fig. 5, the particle size of the nano silver particles in the nano silver powder obtained in this example ranges from 200nm to 600nm, and the particle size distribution is wide, because the increase in temperature accelerates the growth rate of the particle size, but the residue of the protective agent is small (the protective agent in this example is polyvinyl alcohol).
Example 5
(1) 10g of silver nitrate and 8g of polyethylene glycol are weighed and placed in a beaker, 200g of glycerol is added, and the mixture is stirred at room temperature at the speed of 500r/min until solid particles are completely dissolved, so that the silver ion-containing solution is prepared.
(2) At the same time, 0.8g of sodium hydroxide was weighed, added to 50g of deionized water, and stirred at room temperature until completely dissolved to prepare an alkaline solution.
(3) Mixing the silver ion-containing solution and the alkaline solution, transferring the mixed solution into a 500mL hydrothermal reaction kettle, placing the hydrothermal reaction kettle in a drying oven at 200 ℃ for constant-temperature reaction for 3h, and naturally cooling to room temperature. And centrifuging, collecting, washing and drying the reaction product to obtain the nano silver powder.
Scanning analysis is carried out on the nano silver powder by adopting a scanning electron microscope, and an obtained electron microscope image is shown in FIG. 6. As can be seen from fig. 6, the nano silver particles in the nano silver powder obtained in this example have a quasi-spherical structure, a particle diameter ranging from 50nm to 60nm, and a small and uniform particle diameter.
While the invention has been shown and described with reference to certain embodiments, those skilled in the art will understand that: various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (10)
1. The preparation method of the nano silver powder is characterized by comprising the following steps:
dissolving a silver source and a protective agent in polyhydric alcohol to prepare silver-containing solution;
mixing an alkaline solution with a silver-containing solution, and carrying out hydrothermal reaction at a reaction temperature of 120-200 ℃;
and collecting and separating the reaction product to obtain the nano silver powder, wherein the particle size of nano silver particles in the nano silver powder is 50-600 nm.
2. The method of claim 1, wherein the silver source is silver nitrate, silver trifluoroacetate, silver carbonate or silver acetate.
3. The method according to claim 1, wherein the protective agent is at least one of sodium dodecylbenzenesulfonate, polyvinylpyrrolidone, polyvinyl alcohol, oleic acid, polyethylene glycol, n-dodecyl mercaptan, polyacrylic acid, and lauric acid.
4. The method according to claim 1, wherein the polyhydric alcohol is at least one of ethylene glycol, 1, 2-propylene glycol, glycerol, and pentaerythritol; the alkaline solution is sodium hydroxide solution, potassium hydroxide solution, sodium bicarbonate solution, sodium carbonate solution or ammonia water.
5. The method according to claim 2, wherein the mass ratio of the silver source to the protective agent is in the range of 1: (0.25 to 4); the mass ratio of the polyhydric alcohol to the silver source is in the range of 1: (0.01-0.1).
6. The method according to claim 1, wherein the concentration of the alkaline solution is in the range of 0.05 to 2 mol/L.
7. The preparation method according to claim 1, wherein the reaction time of the hydrothermal reaction is 1-12 h.
8. The method according to any one of claims 1 to 7, wherein the reaction product is separated by at least one of filtration, sedimentation, evaporation and centrifugation.
9. The production method according to any one of claims 1 to 7, characterized in that the nano silver powder is washed and dried; the washing method comprises the steps of repeatedly washing the nano silver powder for 3-5 times by adopting absolute ethyl alcohol and/or deionized water; the drying method includes at least one of vacuum drying, natural drying, heat drying and forced air drying.
10. The method according to claim 9, wherein the temperature of the vacuum drying is 20 to 50 ℃.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111673091A (en) * | 2020-06-18 | 2020-09-18 | 宁夏中色新材料有限公司 | Silver powder preparation method with low dispersant content and high conductivity and silver powder |
| CN112705726A (en) * | 2020-12-17 | 2021-04-27 | 暨南大学 | Preparation method of shape-controllable nano silver powder |
| CN113299422A (en) * | 2021-05-07 | 2021-08-24 | 江西师范大学 | Crystalline silicon solar cell front silver paste and preparation method thereof |
| CN113547132A (en) * | 2021-07-29 | 2021-10-26 | 长沙新材料产业研究院有限公司 | Method for preparing nano silver powder by hydrothermal method and nano silver powder |
| CN113770373A (en) * | 2021-09-28 | 2021-12-10 | 长沙新材料产业研究院有限公司 | Nano-silver reaction stock solution, preparation method and nano-silver |
| CN114131035A (en) * | 2021-11-30 | 2022-03-04 | 长沙新材料产业研究院有限公司 | Silver powder preparation method and silver powder |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111673091A (en) * | 2020-06-18 | 2020-09-18 | 宁夏中色新材料有限公司 | Silver powder preparation method with low dispersant content and high conductivity and silver powder |
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| CN112705726A (en) * | 2020-12-17 | 2021-04-27 | 暨南大学 | Preparation method of shape-controllable nano silver powder |
| CN113299422A (en) * | 2021-05-07 | 2021-08-24 | 江西师范大学 | Crystalline silicon solar cell front silver paste and preparation method thereof |
| CN113547132A (en) * | 2021-07-29 | 2021-10-26 | 长沙新材料产业研究院有限公司 | Method for preparing nano silver powder by hydrothermal method and nano silver powder |
| CN113770373A (en) * | 2021-09-28 | 2021-12-10 | 长沙新材料产业研究院有限公司 | Nano-silver reaction stock solution, preparation method and nano-silver |
| CN114131035A (en) * | 2021-11-30 | 2022-03-04 | 长沙新材料产业研究院有限公司 | Silver powder preparation method and silver powder |
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Application publication date: 20200519 |