CN113084184A - Nano silver sheet and preparation method thereof - Google Patents
Nano silver sheet and preparation method thereof Download PDFInfo
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- CN113084184A CN113084184A CN202110319767.0A CN202110319767A CN113084184A CN 113084184 A CN113084184 A CN 113084184A CN 202110319767 A CN202110319767 A CN 202110319767A CN 113084184 A CN113084184 A CN 113084184A
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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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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0551—Flake form nanoparticles
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a nano silver sheet and a preparation method thereof, 40-50ml of silver ammonia solution with the concentration of 0.06-1.2mol/L is taken, 5-10ml of reducing agent and 5-10ml of aluminum nitrate solution with the concentration of 0.1-1.0mol/L are sequentially added under the stirring condition, and the stirring is continued until the reaction is complete at normal temperature; and after the reaction is finished, performing centrifugal separation on the product, washing the product by using deionized water, and performing vacuum drying to obtain the nano silver sheet. Compared with the prior art, the method has the advantages that hydrogen peroxide is used as a reducing agent in the aqueous solution at room temperature to reduce the silver ammonia solution to synthesize the hexagonal silver nanosheets, the method is low in cost, good in stability, simple in synthesis process and reliable in quality, and is suitable for large-scale preparation.
Description
Technical Field
The invention relates to the field of chemical engineering, in particular to a nano silver sheet and a preparation method thereof.
Background
The nano particles are particles with the particle size of 1-100nm, are positioned in a transition region between an atomic cluster and a macroscopic object, are a typical mesoscopic system, and have special surface effect, small-size effect and macroscopic quantum tunneling effect. When the macroscopic object is subdivided into the nano particles, the optical, thermal, electrical, magnetic, mechanical and chemical properties of the macroscopic object can be obviously changed, and the macroscopic object can be widely applied to a plurality of fields such as electronics, medicine, chemical engineering, military, aerospace and the like. These properties and applications are closely related to the morphology and size of the nanoparticles. Therefore, the control of the material performance is realized by adjusting the appearance, the size, the dimension and the composition of the nano particles, and finally, a functional nano device is designed and realized.
The preparation method of the nano silver sheet mainly comprises a reduction ball milling method, a chemical reduction method, a photoinduction method, a template method, a solvothermal method, a microwave radiation method, an ultrasonic auxiliary method and the like. The chemical reduction method is one of the common methods for preparing the nano silver at low cost due to high yield, low cost and simple and convenient operation. However, most chemical methods require the introduction of a large amount of chemical reagents, and have the problems of high production cost, difficulty in removing organic matters in a system, possibility of causing certain environmental pollution and the like.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides the nano silver sheet and the preparation method thereof, wherein the nano silver sheet is simple in process, low in cost and convenient to operate.
In order to achieve the purpose, the invention is implemented according to the following technical scheme:
a preparation method of a nano silver sheet comprises the following steps:
s1, obtaining a silver ammonia solution with the concentration of 0.06-1.2 mol/L;
s2, taking 40-50ml of silver-ammonia solution, sequentially adding 5-10ml of reducing agent and 5-10ml of aluminum nitrate solution with the concentration of 0.1-1.0mol/L under the stirring condition, and continuously stirring at normal temperature until the reaction is complete;
and S3, after the reaction is finished, performing centrifugal separation on the product, washing the product with deionized water, and performing vacuum drying to obtain the nano silver sheet.
As a further preferable embodiment of the present invention, the step S1 of obtaining the silver ammonia solution with the concentration of 0.06-1.2mol/L comprises the following specific steps:
0.408g of silver nitrate is prepared into silver nitrate solution with the concentration of 0.12mol/L by 20ml of water, ammonia water is slowly added and oscillated until sediment is generated, and the ammonia water is continuously added dropwise under the oscillation until the sediment is completely dissolved to prepare clear silver ammonia solution.
In a further preferred embodiment of the present invention, the reducing agent in step S2 is hydrogen peroxide with a concentration of 1 to 30%.
In a further preferred embodiment of the present invention, the step S2 is performed in a magnetic stirrer, and the stirring time is 40-60 min.
As a further preferable scheme of the present invention, the rotation number of the centrifugal separation in the step S3 is 8000-9000r/min, and the centrifugal time is 10-20 min.
The second purpose of the invention is to provide a nano silver sheet prepared by the method.
Compared with the prior art, the invention has the following beneficial effects:
1) the invention adopts hydrogen peroxide as a reducing agent in aqueous solution at room temperature to reduce silver ammonia solution to synthesize the hexagonal silver nanosheet, and the method has the advantages of low cost, good stability, simple synthesis process, reliable quality and large-scale preparation.
2) The reducing agent and the solvent adopted by the invention are nontoxic and pollution-free chemical reagents, and the method has less waste discharge and is an environment-friendly preparation method.
Drawings
FIG. 1 is an X-ray diffraction pattern of the product of example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of the product of example 1 of the present invention, with a 2 μm scale.
FIG. 3 is a scanning electron micrograph of the product of example 1 of the present invention showing 10. mu.mL.
FIG. 4 is a transmission electron micrograph of the product of example 2 of the present invention, with a scale of 1 μm.
FIG. 5 is a scanning electron micrograph of the product of example 2 of the present invention, wherein the scale is 10 μm.
FIG. 6 is a scanning electron micrograph of the product of example 3 of the present invention showing 10. mu.mL.
FIG. 7 is a scanning electron micrograph of the product of example 4 of the present invention, which shows a 10 μm scale.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. The specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Example 1
(1) Weighing 0.408g of silver nitrate and preparing the silver nitrate into a silver nitrate solution with the concentration of 0.12mol/L by using 20ml of water;
(2) weighing 0.302g of aluminum nitrate and preparing the aluminum nitrate solution with the concentration of 0.2mol/L by using 4ml of water;
(3) 5ml (with the concentration of 30 percent) of hydrogen peroxide is added into 45ml of water to prepare a hydrogen peroxide solution with the concentration of 3 percent;
(4) under the condition of room temperature, dropwise adding ammonia water into the solution obtained in the step (1) while stirring until generated precipitates just disappear, and preparing a silver-ammonia solution;
(5) then 5ml of hydrogen peroxide solution with the concentration of 3 percent and aluminum nitrate solution are added into the prepared silver-ammonia solution, and the mixture is stirred for one hour at normal temperature;
(6) and after the reaction is finished, performing centrifugal separation on the product, washing the product by using deionized water, and performing vacuum drying to obtain the nano silver sheet.
The nano silver sheet prepared in this example was subjected to X-ray diffraction phase analysis, and the X-ray diffraction pattern thereof is shown in fig. 1, which was compared with a standard X-ray diffraction pattern of conventional silver, indicating that the prepared product was silver. The characterization of the nano silver sheet prepared in this embodiment by a scanning electron microscope is shown in fig. 2 (2 μm scale) and fig. 3 (10 μm scale), and it can be seen from fig. 2 and fig. 3 that the nano silver sheet prepared in this embodiment has a hexagonal structure.
Example 2
(1) Weighing 0.408g of silver nitrate and preparing the silver nitrate into a silver nitrate solution with the concentration of 0.12mol/L by using 20ml of water;
(2) weighing 0.302g of aluminum nitrate and preparing the aluminum nitrate solution with the concentration of 0.2mol/L by using 4ml of water;
(3) 5ml (with the concentration of 30 percent) of hydrogen peroxide is added into 25ml of water to prepare hydrogen peroxide solution with the concentration of 5 percent;
(4) and (2) dropwise adding ammonia water into the solution obtained in the step (1) under the condition of room temperature while stirring until the generated precipitate just disappears to obtain the silver-ammonia solution.
(5) Then 5ml of 3% hydrogen peroxide and aluminum nitrate solution were added to the prepared silver ammonia solution, and stirred for one hour at normal temperature.
(6) And after the reaction is finished, performing centrifugal separation on the product, washing the product by using deionized water, and performing vacuum drying to obtain the nano silver sheet.
The nano silver sheet prepared in this example is characterized by a scanning electron microscope and a transmission electron microscope as shown in fig. 4 (with a scale of 1 μm) and fig. 5 (with a scale of 10 μm), and as can be seen from fig. 4 and 5, the nano silver sheet prepared in this example has a hexagonal structure.
Example 3
(1) Weighing 0.408g of silver nitrate and preparing the silver nitrate into a silver nitrate solution with the concentration of 0.12mol/L by using 20ml of water;
(2) weighing 0.302g of aluminum nitrate and preparing the aluminum nitrate solution with the concentration of 0.2mol/L by using 4ml of water;
(3) 5ml (with the concentration of 30 percent) of hydrogen peroxide is added into 5ml of water to prepare a hydrogen peroxide solution with the concentration of 15 percent;
(4) and (2) dropwise adding ammonia water into the solution obtained in the step (1) under the condition of room temperature while stirring until the generated precipitate just disappears to obtain the silver-ammonia solution.
(5) Then 5ml of 3% hydrogen peroxide and aluminum nitrate solution were added to the prepared silver ammonia solution, and stirred for one hour at normal temperature.
(6) And after the reaction is finished, performing centrifugal separation on the product, washing the product by using deionized water, and performing vacuum drying to obtain the nano silver sheet.
The nano silver sheet prepared in this example is characterized by a scanning electron microscope as shown in fig. 6 (with a scale of 10 μm), and as can be seen from fig. 6, the nano silver sheet prepared in this example has a hexagonal structure.
Example 4
(1) Weighing 0.408g of silver nitrate and preparing the silver nitrate into a silver nitrate solution with the concentration of 0.12mol/L by using 20ml of water;
(2) weighing 0.151g of aluminum nitrate and preparing the aluminum nitrate solution with the concentration of 0.1mol/L by using 4ml of water;
(3) 5ml (with the concentration of 30 percent) of hydrogen peroxide is added into 45ml of water to prepare hydrogen peroxide solution with the concentration of 5 percent;
(4) and (2) dropwise adding ammonia water into the solution obtained in the step (1) under the condition of room temperature while stirring until the generated precipitate just disappears to obtain the silver-ammonia solution.
(5) Then 5ml of 3% hydrogen peroxide and aluminum nitrate solution were added to the prepared silver ammonia solution, and stirred for one hour at normal temperature.
(6) And after the reaction is finished, performing centrifugal separation on the product, washing the product by using deionized water, and performing vacuum drying to obtain the nano silver sheet.
The nano silver sheet prepared in this example is characterized by a scanning electron microscope as shown in fig. 7 (with a scale of 10 μm), and as can be seen from fig. 7, the nano silver sheet prepared in this example has a hexagonal structure.
The technical solution of the present invention is not limited to the limitations of the above specific embodiments, and all technical modifications made according to the technical solution of the present invention fall within the protection scope of the present invention.
Claims (6)
1. The preparation method of the nano silver sheet is characterized by comprising the following steps:
s1, obtaining a silver ammonia solution with the concentration of 0.06-1.2 mol/L;
s2, taking 40-50ml of silver-ammonia solution, sequentially adding 5-10ml of reducing agent and 5-10ml of aluminum nitrate solution with the concentration of 0.1-1.0mol/L under the stirring condition, and continuously stirring at normal temperature until the reaction is complete;
and S3, after the reaction is finished, performing centrifugal separation on the product, washing the product with deionized water, and performing vacuum drying to obtain the nano silver sheet.
2. The method for preparing nano silver flakes according to claim 1, wherein the step of obtaining the silver ammonia solution with the concentration of 0.06-1.2mol/L in step S1 comprises the following specific steps:
0.408g of silver nitrate is prepared into silver nitrate solution with the concentration of 0.12mol/L by 20ml of water, ammonia water is slowly added and oscillated until sediment is generated, and the ammonia water is continuously added dropwise under the oscillation until the sediment is completely dissolved to prepare clear silver ammonia solution.
3. The method for preparing nano-silver flakes according to claim 1, wherein the reducing agent in step S2 is hydrogen peroxide with a concentration of 1-30%.
4. The method for preparing nano-silver flake according to claim 1, wherein the step S2 is performed in a magnetic stirrer, and the stirring time is 40-60 min.
5. The method as claimed in claim 1, wherein the rotation speed of the centrifugal separation in step S3 is 8000-9000r/min, and the centrifugal time is 10-20 min.
6. A nanosilver sheet prepared by the method of any one of claims 1 to 5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110319767.0A CN113084184A (en) | 2021-03-25 | 2021-03-25 | Nano silver sheet and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116329361A (en) * | 2023-05-19 | 2023-06-27 | 苏州中毅精密科技有限公司 | Method, device, equipment and medium for preparing sheet based on fluid impact |
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| CN1128188A (en) * | 1995-09-29 | 1996-08-07 | 中国科学院固体物理研究所 | Size-controllable preparation method of nanometer-level silver |
| JPH11106806A (en) * | 1997-10-02 | 1999-04-20 | Mitsui Mining & Smelting Co Ltd | Silver powder composed of hexagonal sheet-shaped crystal silver grain and its production |
| CN103350236A (en) * | 2013-07-25 | 2013-10-16 | 湖南科技大学 | Method for compounding hexagon silver nanosheet |
| CN103769601A (en) * | 2014-01-22 | 2014-05-07 | 清华大学 | Preparing method of triangular flaky nanometer silver particles |
| CN109848439A (en) * | 2019-04-09 | 2019-06-07 | 苏州大学 | A kind of preparation method of Nano silver piece |
| KR20200018948A (en) * | 2018-08-13 | 2020-02-21 | 김태관 | Manufacturing method of silver flake |
| CN110899722A (en) * | 2019-12-26 | 2020-03-24 | 无锡晶睿光电新材料有限公司 | Thin single crystal flake silver powder synthesized by chemical method and preparation method thereof |
-
2021
- 2021-03-25 CN CN202110319767.0A patent/CN113084184A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1128188A (en) * | 1995-09-29 | 1996-08-07 | 中国科学院固体物理研究所 | Size-controllable preparation method of nanometer-level silver |
| JPH11106806A (en) * | 1997-10-02 | 1999-04-20 | Mitsui Mining & Smelting Co Ltd | Silver powder composed of hexagonal sheet-shaped crystal silver grain and its production |
| CN103350236A (en) * | 2013-07-25 | 2013-10-16 | 湖南科技大学 | Method for compounding hexagon silver nanosheet |
| CN103769601A (en) * | 2014-01-22 | 2014-05-07 | 清华大学 | Preparing method of triangular flaky nanometer silver particles |
| KR20200018948A (en) * | 2018-08-13 | 2020-02-21 | 김태관 | Manufacturing method of silver flake |
| CN109848439A (en) * | 2019-04-09 | 2019-06-07 | 苏州大学 | A kind of preparation method of Nano silver piece |
| CN110899722A (en) * | 2019-12-26 | 2020-03-24 | 无锡晶睿光电新材料有限公司 | Thin single crystal flake silver powder synthesized by chemical method and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| YI HE等: "A facile route to silver nanosheets", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116329361A (en) * | 2023-05-19 | 2023-06-27 | 苏州中毅精密科技有限公司 | Method, device, equipment and medium for preparing sheet based on fluid impact |
| CN116329361B (en) * | 2023-05-19 | 2023-08-01 | 苏州中毅精密科技有限公司 | Method, device, equipment and medium for preparing sheet based on fluid impact |
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Application publication date: 20210709 |