CN110841890A - Silver nanostructure based on graphene-PVP mixed coating protection and preparation method thereof - Google Patents
Silver nanostructure based on graphene-PVP mixed coating protection and preparation method thereof Download PDFInfo
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- CN110841890A CN110841890A CN201910957805.8A CN201910957805A CN110841890A CN 110841890 A CN110841890 A CN 110841890A CN 201910957805 A CN201910957805 A CN 201910957805A CN 110841890 A CN110841890 A CN 110841890A
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Abstract
The invention discloses a silver nanostructure based on graphene-PVP mixed coating protection and a preparation method thereof. The silver nanostructure protected based on the graphene-PVP mixed coating comprises a silver nanostructure, a polyvinylpyrrolidone (PVP) layer and graphene, wherein the PVP layer is wrapped on the surface of the silver nanostructure and is obtained when the silver nanostructure is synthesized by a polyalcohol method by taking PVP as a surfactant, and the graphene-PVP mixed coating is formed on the surface of the silver nanostructure after graphene transfer. The surface of the silver nanostructure prepared by the method is covered with the graphene-PVP protective layer, so that the silver nanostructure is prevented from contacting with the external environment, the double protection of the silver nanostructure can be realized, the oxidation of the silver nanostructure is inhibited, and the long-term stable use of the silver nanostructure is facilitated.
Description
Technical Field
The invention relates to the technical field of nano materials and corrosion prevention, in particular to a silver nano structure based on protection of a graphene-PVP mixed coating and a preparation method thereof.
Background
With the rapid development of electronic devices, the demand for highly integrated chips is increasingly prominent. The silver nanostructure has the characteristics of small size, high conductivity and the like, and is an ideal material applied to high-integration circuits. The current research shows that the silver nanostructure has important potential application value in the fields of sensing, photoelectric devices, high-integration-level nano electronic networks, flexible transparent conductive films and the like. However, since the silver surface is very easily oxidized, it is greatly limited in practical use. The PVP is taken as a surfactant, and the surface of the silver nano structure prepared by the polyol method is covered by a PVP thin layer, so that the nano silver can be isolated from the external environment, and the silver oxidation is inhibited. However, the research finds that the PVP layer is not enough to effectively inhibit the occurrence of the galvanic corrosion phenomenon for a long time, and the long-term stability of the silver nanostructure cannot be maintained. Therefore, it is desirable to provide a protective layer material that is ultra-thin and has minimal impact on the physical properties of the silver nanostructures themselves, making it a protective coating for the easily oxidizable nanomaterials.
The thickness of the coating obtained by the existing coating technology is thick, and the original physical properties of the metal nano structure are inevitably influenced, so that the metal nano structure is limited to a certain extent. The graphene with the unique properties of atomic layer thickness, excellent chemical stability and high-temperature stability, impermeability to all gases and liquids, and the like, has prominent important application in the field of material corrosion prevention. The graphene is transferred to the surface of the silver nanostructure with the PVP coating, so that the double protection of the silver nanostructure can be realized, the galvanic corrosion phenomenon can be effectively inhibited, and the excellent performance of the silver can be maintained. The method for protecting the silver nano structure based on the graphene-PVP mixed coating is provided, the method for inhibiting the oxidation of the silver nano material is provided, the wide application of the silver nano material is certainly promoted, and the development of subjects such as material science, information, integrated circuits and the like is promoted.
Disclosure of Invention
The invention aims to solve the technical problem of providing a silver nanostructure with a graphene-PVP protective layer covered on the surface and a preparation method thereof aiming at the defects in the prior art.
The invention is realized by the following technical scheme:
a silver nanostructure based on protection of a graphene-PVP mixed coating comprises the silver nanostructure, a polyvinylpyrrolidone (PVP) layer and graphene, wherein the PVP layer is wrapped on the surface of the silver nanostructure and is obtained when the PVP is used as a surfactant to synthesize the silver nanostructure through a polyol method, and the graphene is transferred to form the graphene-PVP mixed coating on the surface of the silver nanostructure.
Further, the molecular weight of the PVP is 38000-55000, and the thickness of the PVP layer on the surface of the silver nanostructure is less than 4 nm.
Further, the substrate is a glass, quartz, silicon wafer, PDMS or PET flexible substrate.
Further, the graphene is prepared by a Chemical Vapor Deposition (CVD) method or a mechanical peeling method.
Further, the number of graphene layers may be a single layer or a plurality of layers.
Further, the silver nano structure comprises silver nanowires, silver nanocubes, silver nanorods, silver nano cuboids, silver nano rice and silver nano pyramids.
A preparation method of a silver nanostructure based on protection of a graphene-PVP mixed coating comprises the following steps:
(1) preparing a silver nanostructure with a PVP thin layer on the surface by using PVP as a surfactant and adopting a polyol method;
(2) washing the silver nanostructure prepared in the step (1) with acetone, ethanol and ultrapure water in sequence, finally dissolving the obtained relatively pure silver nanostructure in ethanol, and stirring to obtain uniform dispersion liquid of the silver nanostructure for subsequent use;
(3) removing impurities on the surface of the substrate by using acetone and isopropanol respectively, then ultrasonically oscillating the substrate in deionized water for 3-5 minutes, blow-drying the substrate by using nitrogen for later use, and then dropwise adding or spin-coating the uniform dispersion liquid of the silver nano structure prepared in the step (2) on the clean surface of the substrate;
(4) transferring graphene to the surface of a substrate coated with silver nanostructures, naturally drying, and then placing the substrate in 10% H2And N2Annealing for 3 hours at the temperature of 150 ℃ and 200 ℃ in the mixed gas.
Compared with the prior art, the invention has the beneficial effects that: the surface of the silver nanostructure is covered with a graphene-PVP protective layer, so that the silver nanostructure is prevented from contacting with the external environment, the double protection of the silver nanostructure can be realized, the oxidation of the silver nanostructure is inhibited, and the long-term stable use of the silver nanostructure is facilitated. In addition, the graphene-PVP protective layer is thin, has the smallest influence on the original physical properties of the silver nanostructure, and is beneficial to wide research and development and application of high-performance devices based on the silver nanostructure. The method has the advantages of simple process and high cost performance, and has good development prospect in the field of nano material anticorrosion application.
Drawings
Fig. 1 is a schematic diagram of a silver nanostructure with a graphene-PVP protective layer.
In the drawings, the reference numerals denote the following components:
1. a substrate; 2. a graphene layer; 3. a layer of polyvinylpyrrolidone (PVP); 4. silver nanostructures.
Detailed Description
The technical solution of the present invention is clearly and completely described below with reference to specific embodiments. It is obvious that the described embodiments are only some of the embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The method for preparing the silver nanowire structure with the PVP as the surface active agent and the PVP layer wrapped on the surface by adopting a polyhydric alcohol method comprises the following specific steps: firstly, 0.1666g and 0.6742g of AgNO are taken3And PVP are respectively dissolved in 6mL of ethylene glycol solution, AgNO3Care should be taken to protect from light during the dissolution process. While preparing two reactant solutions, adding the methyl silicone oil in an oil bath kettleHeating was carried out and when the temperature reached and stabilized at 160 ℃, the flask containing 5mL of ethylene glycol solution was immersed in an oil bath and fixed. Heating is continued for about 10min, so that the temperature of the ethylene glycol solution is kept at 160 ℃. The temperature of the solution in the flask should be kept uniform throughout the heating and reaction process using a condenser and magnetic stirring. Then, the prepared 6mL AgNO was injected by means of a two-channel syringe pump3And PVP solution was simultaneously added dropwise to the ethylene glycol solution at a rate of 0.8 mL/min. Finally, the mixed solution was further heated at 160 ℃ for 40 min. And sequentially washing the obtained product with acetone, ethanol and ultrapure water for 2 times respectively, and finally dissolving the obtained pure silver nanowire structure in the ethanol for subsequent use. Respectively soaking the silicon wafer substrate in acetone and isopropanol for 3 minutes to remove impurities on the surface of the silicon wafer substrate, then ultrasonically oscillating the silicon wafer in deionized water for 3 minutes, and drying the silicon wafer by nitrogen for later use. Placing the uniform dispersion liquid containing the silver nanowire structure on the surface of a clean silicon wafer substrate. Finally, 1X 1cm2The CVD graphene is transferred to the surface of the silicon wafer substrate structure, and the specific process is as follows: first, a PMMA solution was spin-coated on the surface of a copper foil on which graphene was grown by a CVD method, using a plasma cleaner (gas: Ar/O)2And the cleaning time is as follows: 20s) removing pollutants and oxides on the back surface (the surface without graphene) of the copper foil; then etching the copper foil by using 25g/L ammonium persulfate solution; repeatedly washing the graphene coated with the PMMA layer for multiple times by using deionized water; then transferring the silver-containing nanowire structure to the surface of a silicon wafer substrate with the silver-containing nanowire structure, and naturally airing; it was then placed in 10% H2And N2Annealing for 3 hours at 200 ℃ in the mixed gas; and finally, respectively soaking the graphene layer in acetone and isopropanol for 3 minutes to remove the PMMA layer coated on the graphene, and naturally airing.
Example 2
The preparation method comprises the following steps of preparing a silver nanocube structure with a PVP layer wrapped on the surface by using PVP as a surfactant and adopting a polyol method: the oil bath pan was preheated to 160 ℃. Meanwhile, three solutions each using ethylene glycol as a solvent were prepared. Solution one was 30. mu.l of 13.6mM sodium bromide (NaBr) solution and solution two was 27mL of 94mM AgNO3Solution III is 135mL of 144mM PVP and 0.144mM NaBr. It is noted that AgNO3Easily decomposed by light, and containing AgNO3Care should be taken to avoid light. After the completion of the preparation, 5mL of an ethylene glycol solution was added to the one-necked flask, which was then placed in an oil bath pan and heated so that the temperature of the ethylene glycol solution was stabilized at 160 ℃. In the whole experimental process, the single-neck flask always uses the condenser tube to carry out cooling reflux, and the inside of the flask always uses the cylindrical magneton to keep magnetic stirring. After heating for 10min, 30. mu.L of the first solution was added dropwise to the single-necked flask using a pipette, then 3.2mL of the second solution and the same volume of the third solution were simultaneously added dropwise to the single-necked flask at a rate of 0.375mL/min by means of a two-channel syringe pump, and the reaction was terminated after continuous heating at 160 ℃ for 40 min. And sequentially washing the obtained product with acetone, ethanol and ultrapure water for 2 times respectively, and finally dissolving the obtained pure silver nanocube structure in ethanol for subsequent use. And ultrasonically oscillating the cured PDMS substrate in ethanol for 3 minutes, and drying the PDMS substrate by nitrogen for later use. The silver-containing nanocube structured uniform dispersion was placed on the clean PDMS substrate surface. Finally, 1X 1cm2The CVD graphene is transferred to the surface of the PDMS substrate structure, and the specific process is as follows: first, a PMMA solution was spin-coated on the surface of a copper foil on which graphene was grown by a CVD method, using a plasma cleaner (gas: Ar/O)2And the cleaning time is as follows: 20s) removing pollutants and oxides on the back surface (the surface without graphene) of the copper foil; then etching the copper foil by using 25g/l ammonium persulfate solution; repeatedly washing the graphene coated with the PMMA layer for multiple times by using deionized water; then transferring the silver-containing nano cubic structure to the surface of a PDMS substrate with the silver-containing nano cubic structure, and naturally airing; it was then placed in 10% H2And N2Annealing the graphene oxide film in the mixed gas for 3 hours at the temperature of 150 ℃, finally respectively soaking the graphene oxide film in acetone and isopropanol for 3 minutes to remove the PMMA layer coated on the graphene, and naturally airing the graphene oxide film.
Claims (7)
1. The silver nanostructure based on protection of the graphene-PVP mixed coating is characterized by comprising the silver nanostructure, a polyvinylpyrrolidone (PVP) layer and graphene, wherein the PVP layer is wrapped on the surface of the silver nanostructure and is obtained when the silver nanostructure is synthesized by a polyol method by taking PVP as a surfactant, and the graphene-PVP mixed coating is formed on the surface of the silver nanostructure after graphene transfer.
2. The graphene-PVP mixed coating protection-based silver nanostructure according to claim 1, wherein the molecular weight of PVP is 38000-55000, and the thickness of PVP layer on the surface of the silver nanostructure is less than 4 nm.
3. The graphene-PVP hybrid coating protection-based silver nanostructure according to claim 1, wherein the substrate is a glass, quartz, silicon wafer, PDMS or PET flexible substrate.
4. The graphene-PVP hybrid coating protection-based silver nanostructure of claim 1, wherein the graphene is prepared by a Chemical Vapor Deposition (CVD) method or a mechanical exfoliation method.
5. The silver nanostructure protected based on a graphene-PVP mixed coating according to claim 1, characterized in that the number of graphene layers can be single-layer or multi-layer.
6. The graphene-PVP hybrid coating protection-based silver nanostructure according to claim 1, wherein the silver nanostructure is silver nanowire, silver nanocube, silver nanorod, silver nano-cuboid or silver nano-double pyramid.
7. The method for preparing the silver nanostructure protected on the basis of the graphene-PVP mixed coating according to any one of claims 1-6, wherein the method comprises the following steps:
(1) preparing a silver nanostructure with a PVP thin layer on the surface by using PVP as a surfactant and adopting a polyol method;
(2) washing the silver nanostructure prepared in the step (1) with acetone, ethanol and ultrapure water in sequence, finally dissolving the obtained relatively pure silver nanostructure in ethanol, and stirring to obtain uniform dispersion liquid of the silver nanostructure for subsequent use;
(3) removing impurities on the surface of the substrate by using acetone and isopropanol respectively, then ultrasonically oscillating the substrate in deionized water for 3-5 minutes, drying the substrate by using nitrogen for later use, and then dropwise adding, spin-coating or printing the uniform dispersion liquid of the silver nano structure prepared in the step (2) on the clean surface of the substrate;
(4) transferring graphene to the surface of a substrate containing the silver nanostructure, naturally drying, and then placing the substrate in 10% H2And N2Annealing at 150-200 ℃ for 3h in the mixed gas.
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Cited By (3)
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| CN112108346A (en) * | 2020-09-24 | 2020-12-22 | 西安工程大学 | Anticorrosive coating for nano metal and preparation method thereof |
| CN113029404A (en) * | 2021-03-10 | 2021-06-25 | 电子科技大学 | Preparation method of dual-channel flexible polymorphic stress sensor based on graphene |
| CN114974932A (en) * | 2022-05-31 | 2022-08-30 | 浙江理工大学 | Preparation method of silver-coated flexible composite film electrode based on sodium polystyrene sulfonate-polyaniline |
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| CN112108346A (en) * | 2020-09-24 | 2020-12-22 | 西安工程大学 | Anticorrosive coating for nano metal and preparation method thereof |
| CN113029404A (en) * | 2021-03-10 | 2021-06-25 | 电子科技大学 | Preparation method of dual-channel flexible polymorphic stress sensor based on graphene |
| CN114974932A (en) * | 2022-05-31 | 2022-08-30 | 浙江理工大学 | Preparation method of silver-coated flexible composite film electrode based on sodium polystyrene sulfonate-polyaniline |
| CN114974932B (en) * | 2022-05-31 | 2023-12-29 | 浙江理工大学 | Preparation method of silver-coated flexible composite film electrode based on sodium polystyrene sulfonate-polyaniline |
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Application publication date: 20200228 |