CN112355321A - Preparation method of kelp-like silver structure - Google Patents

Preparation method of kelp-like silver structure Download PDF

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Publication number
CN112355321A
CN112355321A CN202011074434.8A CN202011074434A CN112355321A CN 112355321 A CN112355321 A CN 112355321A CN 202011074434 A CN202011074434 A CN 202011074434A CN 112355321 A CN112355321 A CN 112355321A
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mixed solution
silver
kelp
silicon wafer
preparation
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CN112355321B (en
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卢涵
金名亮
水玲玲
周国富
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Zhaoqing South China Normal University Optoelectronics Industry Research Institute
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Zhaoqing South China Normal University Optoelectronics Industry Research Institute
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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
    • 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
    • B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
    • 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

Abstract

The invention belongs to the technical field of nano-silver preparation, and discloses a preparation method of a kelp-shaped nano-silver structure, which comprises the following steps: s1, preparing a mixed solution of hydrofluoric acid, silver nitrate and SDS; s2, soaking the cleaned silicon wafer in the mixed solution prepared in the S1 for reaction for a period of time; s3, after the reaction, cleaning the silicon wafer, and drying the silicon wafer to obtain the kelp-shaped nano silver structure; wherein the concentration of the hydrofluoric acid in the mixed solution in the step S1 is 10‑610M, the concentration of silver nitrate in the mixed solution is 10‑61M SDS concentration of 10 in the mixed solution‑6The method is simple to operate, low in cost, simple and convenient in process and convenient for preparing the nano silver structure with the novel kelp shape.

Description

Preparation method of kelp-like silver structure
Technical Field
The invention belongs to the technical field of nano-silver preparation, and particularly relates to a preparation method of a kelp-shaped silver structure.
Background
The silver micro-nano structure is excited through resonance and generates a strong coupling effect with visible light, namely surface plasmon resonance. Based on surface plasmon resonance, the silver micro-nano structure can be widely applied to the fields of catalysis, energy, sensing and the like. It has been demonstrated that surface plasmon resonance depends largely on the size and morphology of silver micro-nano structures.
The common silver structure at present has the shapes of flakes, lines, spheres, triangles, cubes, octahedrons and the like. The prior art has no sea-tangle silver micro-nano structure.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a preparation method of a kelp-like silver structure, which has simple steps and low cost.
The second purpose of the invention is to provide the kelp-like silver structure obtained by the method.
A third object of the present invention is to provide the use of the above sea-tangle-like silver structure.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of a kelp-shaped nano silver structure comprises the following steps:
s1, preparing a mixed solution of hydrofluoric acid, silver nitrate and SDS;
s2, soaking the cleaned silicon wafer in the mixed solution prepared in the S1 for reaction for a period of time;
s3, after the reaction, cleaning the silicon wafer, and drying the silicon wafer to obtain the kelp-shaped nano silver structure;
wherein the concentration of the hydrofluoric acid in the mixed solution in the step S1 is 10-610M, the concentration of silver nitrate in the mixed solution is 10-61M SDS concentration of 10 in the mixed solution-6～1M。
Preferably, in step S1, the concentration of hydrofluoric acid in the mixed solution is 0.05-5M, the concentration of silver nitrate in the mixed solution is 0.0005-0.6M, and the concentration of SDS in the mixed solution is 0.001-0.1M.
Preferably, the reaction time in step S2 is 0.5-30 min.
More preferably, the reaction time in step 2 is 5 min.
The invention also provides application of the sea-tangle-shaped nano silver structure.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a preparation method of a kelp-shaped nano silver structure, which comprises the following steps: s1, preparing a mixed solution of hydrofluoric acid, silver nitrate and SDS; s2, soaking the cleaned silicon wafer in the mixed solution prepared in the S1 for reaction for a period of time; s3, after the reaction, cleaning the silicon wafer, and drying the silicon wafer to obtain the kelp-shaped nano silver structure; wherein the concentration of the hydrofluoric acid in the mixed solution in the step S1 is 10-610M, the concentration of silver nitrate in the mixed solution is 10-61M SDS concentration of 10 in the mixed solution-6The method is simple to operate, low in cost, simple and convenient in process and convenient for preparing the nano silver structure with the novel kelp shape.
Drawings
FIG. 1 is a scanning electron micrograph of a silver structure in the form of a kelp prepared in example 1;
FIG. 2 is a scanning electron micrograph of a silver structure in the form of a kelp prepared in example 2;
FIG. 3 is a scanning electron micrograph of a silver structure in the form of a kelp prepared in example 3;
fig. 4 is a scanning electron micrograph of a silver structure prepared in the comparative example.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The test methods used in the following examples and experimental examples are conventional methods unless otherwise specified; the materials, reagents and the like used, unless otherwise specified, are commercially available reagents and materials; the equipment used, unless otherwise specified, is conventional laboratory equipment.
Example 1
A preparation method of a kelp-like silver structure comprises the following steps:
s1, preparing a mixed solution of 0.75M hydrofluoric acid, 0.03M silver nitrate and 0.005M SDS;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
and S3, reacting for 5min, washing the silicon wafer clean, and drying by nitrogen.
Preparing the kelp-shaped silver structure according to the steps, and taking a scanning electron microscope image of the kelp-shaped silver structure as shown in figure 1.
Example 2
A preparation method of a kelp-like silver structure comprises the following steps:
s1, preparing a mixed solution of 0.75M hydrofluoric acid, 0.03M silver nitrate and 0.01M SDS;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
and S3, reacting for 5min, washing the silicon wafer clean, and drying by nitrogen.
Preparing the kelp-shaped silver structure according to the steps, and taking a scanning electron microscope image of the kelp-shaped silver structure as shown in figure 2.
Example 3
A preparation method of a kelp-like silver structure comprises the following steps:
s1, preparing a mixed solution of 0.75M hydrofluoric acid, 0.03M silver nitrate and 0.03M SDS;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
and S3, reacting for 5min, washing the silicon wafer clean, and drying by nitrogen.
Preparing the kelp-shaped silver structure according to the steps, and taking a scanning electron microscope image of the kelp-shaped silver structure as shown in FIG. 3.
Example 4
A preparation method of a kelp-like silver structure comprises the following steps:
s1, preparing a mixed solution of 0.25M hydrofluoric acid, 0.03M silver nitrate and 0.03M SDS;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
and S3, reacting for 2min, washing the silicon wafer clean, and drying by nitrogen.
The sea-tangle-like silver structure was prepared according to the above procedure.
Example 5
A preparation method of a kelp-like silver structure comprises the following steps:
s1, preparing a mixed solution of 1M hydrofluoric acid, 0.06M silver nitrate and 0.015M SDS;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
and S3, reacting for 3min, washing the silicon wafer clean, and drying by nitrogen.
The sea-tangle-like silver structure was prepared according to the above procedure.
Example 6
A preparation method of a kelp-like silver structure comprises the following steps:
s1, preparing a mixed solution of 5M hydrofluoric acid, 0.6M silver nitrate and 0.02M SDS;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
s3, reacting for 0.5min, washing the silicon wafer clean, and drying by nitrogen.
The sea-tangle-like silver structure was prepared according to the above procedure.
Example 7
A preparation method of a kelp-like silver structure comprises the following steps:
s1, preparing a mixed solution of 0.5M hydrofluoric acid, 1M silver nitrate and 1M SDS;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
and S3, reacting for 10min, washing the silicon wafer clean, and drying by nitrogen.
The sea-tangle-like silver structure was prepared according to the above procedure.
Example 8
A preparation method of a kelp-like silver structure comprises the following steps:
s1, preparing a mixed solution of 1M hydrofluoric acid, 0.3M silver nitrate and 0.00005M SDS;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
and S3, reacting for 30min, washing the silicon wafer clean, and drying by nitrogen.
The sea-tangle-like silver structure was prepared according to the above procedure.
Example 9
A preparation method of a kelp-like silver structure comprises the following steps:
s1, preparing a mixed solution of 5M hydrofluoric acid, 0.6M silver nitrate and 0.1M SDS;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
and S3, reacting for 1min, washing the silicon wafer clean, and drying by nitrogen.
The sea-tangle-like silver structure was prepared according to the above procedure.
Example 10
A preparation method of a kelp-like silver structure comprises the following steps:
s1, preparing a mixed solution of 0.05M hydrofluoric acid, 0.0005M silver nitrate and 0.005M SDS;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
and S3, reacting for 15min, washing the silicon wafer clean, and drying by nitrogen.
The sea-tangle-like silver structure was prepared according to the above procedure.
Comparative example 1
A preparation method of a kelp-like silver structure comprises the following steps:
s1, preparing a mixed solution of 0.75M hydrofluoric acid and 0.03M silver nitrate;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
and S3, reacting for 5min, washing the silicon wafer clean, and drying by nitrogen.
The sea-tangle-like silver structure could not be prepared according to the above procedure, and fig. 4 is a scanning electron micrograph of the prepared silver dendrite structure.
Comparative example 2
A preparation method of a kelp-like silver structure comprises the following steps:
s1, preparation 10-8A mixed solution of M hydrofluoric acid, 0.03M silver nitrate and 0.005M SDS;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
and S3, reacting for 5min, washing the silicon wafer clean, and drying by nitrogen.
The sea-tangle-shaped silver structure could not be prepared according to the above procedure, and fig. 4 is a scanning electron micrograph of the prepared silver particles.
Comparative example 3
A preparation method of a kelp-like silver structure comprises the following steps:
s1, 0.75M hydrofluoric acid is prepared, 10-7A mixed solution of M silver nitrate and 0.005M SDS;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
and S3, reacting for 5min, washing the silicon wafer clean, and drying by nitrogen.
The sea-tangle-like silver structure cannot be prepared according to the above procedure.
Comparative example 4
A preparation method of a kelp-like silver structure comprises the following steps:
s1, preparing 0.75M hydrofluoric acid, 0.03M silver nitrate and 10-9A mixed solution of M SDS;
s2, soaking the silicon wafer in the mixed solution prepared in the step S1;
and S3, reacting for 5min, washing the silicon wafer clean, and drying by nitrogen.
The sea-tangle-like silver structure cannot be prepared according to the above procedure.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.

Claims (4)

1. The preparation method of the kelp-shaped nano silver structure is characterized by comprising the following steps of:
s1, preparing a mixed solution of hydrofluoric acid, silver nitrate and SDS;
s2, soaking the cleaned silicon wafer in the mixed solution prepared in the S1 for reaction for a period of time;
s3, after the reaction, cleaning the silicon wafer, and drying the silicon wafer to obtain the kelp-shaped nano silver structure;
wherein the concentration of the hydrofluoric acid in the mixed solution in the step S1 is 10-610M, the concentration of silver nitrate in the mixed solution is 10-61M SDS concentration of 10 in the mixed solution-6～1M。
2. The method of claim 1, wherein the concentration of hydrofluoric acid in the mixed solution is 0.05-5M, the concentration of silver nitrate in the mixed solution is 0.0005-0.6M, and the concentration of SDS in the mixed solution is 0.001-0.1M in the step S1.
3. The method for preparing the laminaria-like nanosilver structure of claim 1, wherein the reaction time in step S2 is 0.5-30 min.
4. Use of the sea-tangle-like nanosilver structure of any one of claims 1 to 3.
CN202011074434.8A 2020-10-09 2020-10-09 Preparation method of kelp-like silver structure Active CN112355321B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102974837A (en) * 2012-11-29 2013-03-20 江苏技术师范学院 Preparation method for flaky nanometer silver powder
CN104194004A (en) * 2014-01-27 2014-12-10 武汉纺织大学 A green synthesis method of a nanometer silver-sodium alginate composition
CN106041115A (en) * 2016-05-26 2016-10-26 华南理工大学 Sodium alga acid/silver nanowire sol and preparation method thereof
CN107661986A (en) * 2017-08-03 2018-02-06 昆明贵金属研究所 A kind of method for being prepared on a large scale the high sphericity super fine silver powder of high dispersive
CN108220933A (en) * 2017-12-28 2018-06-29 肇庆市华师大光电产业研究院 A kind of preparation method of the surface enhanced Raman scattering substrate of high sensitivity

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102974837A (en) * 2012-11-29 2013-03-20 江苏技术师范学院 Preparation method for flaky nanometer silver powder
CN104194004A (en) * 2014-01-27 2014-12-10 武汉纺织大学 A green synthesis method of a nanometer silver-sodium alginate composition
CN106041115A (en) * 2016-05-26 2016-10-26 华南理工大学 Sodium alga acid/silver nanowire sol and preparation method thereof
CN107661986A (en) * 2017-08-03 2018-02-06 昆明贵金属研究所 A kind of method for being prepared on a large scale the high sphericity super fine silver powder of high dispersive
CN108220933A (en) * 2017-12-28 2018-06-29 肇庆市华师大光电产业研究院 A kind of preparation method of the surface enhanced Raman scattering substrate of high sensitivity

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