CN115488347A - Preparation method of multilayer silver nanosheet - Google Patents
Preparation method of multilayer silver nanosheet Download PDFInfo
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- CN115488347A CN115488347A CN202211101341.9A CN202211101341A CN115488347A CN 115488347 A CN115488347 A CN 115488347A CN 202211101341 A CN202211101341 A CN 202211101341A CN 115488347 A CN115488347 A CN 115488347A
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- multilayer silver
- ethanol
- silver
- agno
- nanosheets
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 36
- 239000004332 silver Substances 0.000 title claims abstract description 36
- 239000002135 nanosheet Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 21
- 101710134784 Agnoprotein Proteins 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 4
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims 15
- 238000004519 manufacturing process Methods 0.000 claims 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 229960000583 acetic acid Drugs 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 229910001867 inorganic solvent Inorganic materials 0.000 description 1
- 239000003049 inorganic solvent Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- -1 silver ions Chemical class 0.000 description 1
- 229940083025 silver preparation Drugs 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
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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
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a method for preparing multilayer silver nanosheets, which comprises the following steps: preparing AgNO with a certain concentration at room temperature 3 Ethanol/water solution; then, to AgNO 3 Adding HF structure directing agent with the same mass and enough FeSO into the ethanol/water solution 4 Reducing agent to form mixed solution and reacting for a period of time; and finally, centrifuging, acid washing and drying the product to obtain the multilayer silver nanosheet. The invention provides a method for preparing multilayer silver nanosheets, which is simple and convenient to operate, good in stability, good in repeatability and high in yield, and is suitable for large-scale production of the multilayer silver nanosheets.
Description
Technical Field
The invention relates to the field of metal silver preparation, in particular to a method for preparing silver by using FeSO 4 Reducing AgNO 3 The method of (3) obtaining a multilayer silver nanoplate.
Background
The nano silver has wide application field. It is an important conductive medium of high-performance conductive paint, is a basic material of a flexible circuit board, a contact switch, a membrane switch and the like, and is also a material of various high-end electrodes and electromagnetic compatibility.
The application performance of the nano silver is closely related to the shape structure of the nano silver. The silver nanosheets have excellent performances in the aspects of conductivity, optical property, antibacterial property, chemical stability, plasticity and the like due to the unique size and shape, and are widely applied to the fields of chemical catalysis, inorganic ion detection, surface Raman enhancement, printing, optoelectronic devices, biological engineering and the like. Therefore, the preparation of silver nanoplates has become a focus of research in recent years.
Liu Chunyan (CN 100531975C) adopts chemical reduction method under acidic condition, uses water as dispersion medium, uses glucose or ascorbic acid reducing agent to directly reduce silver nitrate in solution, uses nitric acid or glacial acetic acid as morphology regulator, and prepares flake micron silver. Yang Hongwei (CN 114589312A) polyvinylpyrrolidone (PVP) and silver nitrate (AgNO) 3 ) And the metal halide is dissolved in the reducing agent solution in sequence and fully mixed, transferred into a high-pressure reaction kettle and reacted for a period of time to obtain the round silver nanosheet. Shen Peipei (CN 110076349B) uses micromolecule organic acid and polyethylene glycol to construct a mixed solution reaction system, and water-soluble silverSalt is used as a silver source, and micromolecular polyphenol compounds in tea extract and a mixture thereof are used as reducing agents to prepare the petal-shaped silver nanosheets. Lai Wenzhong (CN 110253033A) in silver source AgNO 3 And adding a surfactant and a protective agent into the mixed solution of the solution and the trisodium citrate solution, then slowly injecting a reducing agent hydrazine solution into the mixed solution at room temperature under the condition of light source induction by using an injector, and reacting for a period of time to obtain the triangular silver nanosheet. Lai Yuekun (CN 109848439B) sequentially dissolving dopamine, copper sulfate and hydrogen peroxide in Tris buffer solution, mechanically stirring for a certain time, centrifuging to obtain polydopamine, dripping polydopamine solution into a mixed solution of silver nitrate and copper sulfate, and mechanically stirring for a certain time to obtain silver nanosheets.
Therefore, the prior art can be used for preparing micro-nano silver with various shapes and structures; however, in the prior art, a preparation method for multilayer silver nanosheets is still relatively lacking.
Disclosure of Invention
The invention aims to: the preparation method of the multilayer silver nanosheet is provided, and the large-scale production of the multilayer silver nanosheet is realized.
The technical solution of the invention is as follows: at room temperature, in AgNO 3 Using alcohol/AgNO in aqueous solution 3 Homogeneous quantity of HF structure directing agent and sufficient FeSO 4 And (4) reducing agent to obtain the multilayer silver nanosheet.
The preparation method of the multilayer silver nanosheet comprises the following specific steps:
(1) Preparing a certain concentration of AgNO at room temperature 3 Ethanol/water solution;
(2) To AgNO 3 Adding HF structure directing agent and sufficient reducing agent FeSO with the same mass into the ethanol/water solution 4 Forming a mixed solution, and reacting for a period of time;
(3) And centrifuging, acid washing and drying the obtained product to obtain the multilayer silver nanosheet.
In step (1), the AgNO 3 The concentration of the ethanol/water solution is 0.01 to 0.03 mol/L, wherein the volume ratio of the ethanol/water is 1/9~3/7.
In the step (2), the sufficient reducing agent FeSO 4 In an amount of AgNO 3 100 to 200 times of the mass.
In the step (2), the reaction time is 45 to 60 minutes.
In the step (3), the product is washed by 0.1 mol/L acetic acid after acid washing.
The principle of the invention is as follows: feSO 4 Has weak reducibility, and can reduce silver ions into silver simple substance. In the reaction system of the invention, feSO is increased 4 The concentration of (A) can accelerate the reduction rate, and is beneficial to the formation of multilayer silver nanosheets; agNO 3 The proper amount of ethanol added into the ethanol/water solution changes the physical and chemical properties of the solution and promotes the growth of the multilayer silver nanosheets. Addition of the same amounts of HF, F - Will be mixed with Ag + Coordination and complexation, and then the dynamic process of the reaction is regulated and controlled. In the reaction system, the silver crystal nucleus formed in the initial stage is influenced by the silver self-structure and can be spontaneously assembled into the single-layer nano sheet, and due to the influence of HF hydrogen bonds or the high surface energy action of the nano sheet, the re-formed silver crystal nucleus can be continuously generated on the single-layer nano sheet to form the multilayer silver nano sheet. Synchronous and accurate control of FeSO4, ethanol and HF reaction concentrations is realized, and the dynamic and thermodynamic stable growth of the multilayer silver nanosheets is realized.
Compared with the prior art, the invention has the following beneficial effects:
1. at room temperature, the large-scale production of the multilayer silver nanosheets can be realized only by means of a simple inorganic solvent.
2. Regulation and control of FeSO 4 The concentration or the volume ratio of ethanol to water in the solution can also realize the layer number adjustment of the silver nanosheets.
3. The method has the advantages of simple operation, good stability, good repeatability and high yield.
Drawings
Fig. 1 a scanning electron microscope picture of multilayer silver nanoplates of example 1.
Fig. 2 scanning electron microscope picture of multilayer silver nanoplates of example 2.
Fig. 3a scanning electron microscope picture of multilayer silver nanoplates of example 3.
Detailed Description
The following examples are provided to further illustrate the technical solutions of the present invention, but should not be construed as limiting the technical solutions.
Example 1: preparing multilayer silver nano-sheet according to the following specific steps
(1) Preparing 0.01 mol/L AgNO at room temperature 3 An ethanol/water solution, wherein the volume ratio of ethanol/water is 1/9;
(2) To AgNO 3 Adding HF structure directing agent with the same mass and AgNO into ethanol/water solution 3 100 times of reducing agent FeSO by mass 4 Forming a mixed solution, and reacting for 45 minutes;
(3) Centrifuging, acid-washing and drying the obtained product to obtain multilayer silver nanosheets; the product obtained by acid washing is washed by 0.1 mol/L acetic acid.
Example 2: preparing multilayer silver nano-sheet according to the following specific steps
(1) Preparing 0.02 mol/L AgNO at room temperature 3 An ethanol/water solution, wherein the volume ratio of ethanol/water is 1/7;
(2) To AgNO 3 Adding HF structure directing agent with the same mass and AgNO into ethanol/water solution 3 150 times of mass of reducing agent FeSO 4 Forming a mixed solution, and reacting for 48 minutes;
(3) Centrifuging, acid washing and drying the product to obtain multilayer silver nanosheets; the product of the acid washing is washed by 0.1 mol/L acetic acid.
Example 3: preparing multilayer silver nano-sheet according to the following specific steps
(1) Preparing 0.03 mol/L AgNO at room temperature 3 An ethanol/water solution, wherein the volume ratio of ethanol/water is 3/7;
(2) To AgNO 3 Adding HF structure directing agent with the same mass and AgNO into ethanol/water solution 3 200 times of mass of reducing agent FeSO 4 Forming a mixed solution, and reacting for 60 minutes;
(3) Centrifuging, acid-washing and drying the obtained product to obtain multilayer silver nanosheets; the product of the acid washing is washed by 0.1 mol/L acetic acid.
Claims (6)
1. A preparation method of multilayer silver nanosheets is characterized by comprising the following steps: and (3) obtaining the multilayer silver nanosheets by using HF structure directing agent with the same mass as AgNO3 and sufficient FeSO4 reducing agent in AgNO3 ethanol/water solution at room temperature.
2. The preparation method of multilayer silver nanosheets as claimed in claim 1, characterized in that it comprises the following specific steps:
(1) Preparing AgNO3 ethanol/water solution with certain concentration at room temperature;
(2) Adding HF structure directing agent with the same mass and sufficient reducing agent FeSO4 into AgNO3 ethanol/water solution to form mixed solution, and reacting for a period of time;
(3) And centrifuging, acid washing and drying the obtained product to obtain the multilayer silver nanosheet.
3. A method of making multilayer silver nanoplates as defined in claim 2, characterised in that: in the step (1), the concentration of the AgNO3 ethanol/water solution is 0.01 to 0.03 mol/L, wherein the volume ratio of ethanol/water is 1/9~3/7.
4. A method of making multilayer silver nanoplates as defined in claim 2, characterised in that: in the step (2), the amount of the sufficient reducing agent FeSO4 is 100 to 200 times of the mass of AgNO 3.
5. A method of preparing multilayer silver nanoplates as claimed in claim 2, characterised in that: in the step (2), the reaction is carried out for 45 to 60 minutes.
6. A method of making multilayer silver nanoplates as defined in claim 2, characterised in that: in the step (3), the product is washed by 0.1 mol/L acetic acid after acid washing.
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| CN202211101341.9A CN115488347B (en) | 2022-09-09 | 2022-09-09 | Preparation method of multilayer silver nano-sheet |
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