CN107014799B - Graphene/silver nanoflower/PMMA sandwich structure flexible SERS substrate and preparation method thereof - Google Patents
Graphene/silver nanoflower/PMMA sandwich structure flexible SERS substrate and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene/silver nanoflower/PMMA sandwich structure flexible SERS substrate and a preparation method thereof, which solve the problems that in the prior art, a rigid substrate of SERS is difficult to adapt to various different surface appearances, a noble metal nano structure cannot be tightly combined with the substrate, and the noble metal nano structure is easy to oxidize. The specific scheme is as follows: the flexible SERS substrate comprises single-layer graphene, a silver nanoflower layer growing on the surface of the single-layer graphene and a PMMA thin film covering the surface of the silver nanoflower layer, so that the silver nanoflower layer is sandwiched between the single-layer graphene and the PMMA thin film.
Description
Technical Field
The invention belongs to the field of preparation of flexible SERS substrates, and particularly relates to a graphene/silver nanoflower/PMMA sandwich-structured flexible SERS substrate and a preparation method thereof.
Background
Surface Enhanced Raman Scattering (SERS) has attracted wide attention since the past because it can effectively amplify intrinsic raman signals and achieve ultrasensitive single-molecule detection, and is gradually applied to a variety of fields such as chemical detection, food safety, and environmental monitoring. The SERS mechanism is widely accepted to be both physical enhancement, mainly due to electric field enhancement caused by surface plasmon resonance, and chemical enhancement, mainly due to charge exchange between the substrate and the molecule. Generally, the rough noble metal surface and noble metal nanostructures are primarily physical enhancements, while the noble metal planes, some semiconductors, and novel two-dimensional layered materials are primarily chemical enhancements. The SERS substrate combining the two enhancement principles is a hot spot in research.
In recent years, studies show that graphene has a SERS effect based on chemical enhancement, and graphene itself has many advantages: (1) due to good biomolecule affinity of graphene, the graphene can be used as a biomolecule enrichment layer; (2) graphene based chemically enhanced SERS effect allows graphene to act as an additional enhancement layer; (3) due to good chemical inertia of the graphene, the graphene can be used as a natural protective layer of a noble metal nano structure; (4) the property of graphene to quench fluorescence makes it possible to act as a fluorescence quenching layer. The method for manufacturing the composite SERS substrate by combining the graphene and the metal nano structure is a hotspot field of research in recent years and obtains good results. Most SERS substrates are rigid substrates, and the rigid material substrates which cannot be bent are difficult to adapt to various surface morphologies and difficult to perform in-situ trace detection on substances. Noble metal nanostructures (gold, silver, copper, etc.) on rigid substrates are typically prepared and then transferred to rigid substrates. However, the process of preparing the graphene-metal nanostructure composite SERS substrate by the transfer method is extremely complex, and the close combination of the graphene-metal nanostructure cannot be realized by physical compounding, and the traditional precious metal nanostructure is generally a nanoparticle, so that the signal enhancement effect of the nanoparticle is poor, and the detection sensitivity is limited. Furthermore, the problem of oxidation of the noble metal nanostructures used (gold, silver, copper, etc.) is also one of the problems that is difficult to overcome.
In summary, the rigid substrate of SERS in the prior art is difficult to adapt to various surface morphologies, the noble metal nanostructure cannot be tightly bonded to the substrate, and the noble metal nanostructure is easily oxidized, and an effective solution is not available at present.
Disclosure of Invention
Flexible SERS substrates have many rare advantages, such as: the flexible SERS substrate can be attached to the outer surfaces of objects in different shapes to perform in-situ detection of Raman signals, and the SERS flexible substrate with good light transmittance can be placed on the surface of a liquid to perform nondestructive Raman signal detection. The advantages enable the flexible SERS substrate to have strong practical applicability and great potential for carrying out in-situ trace detection on real objects.
Although graphene has not been used for the preparation of the flexible SERS substrate at present, the flexibility of graphene makes it possible to be a material for the flexible SERS substrate, so the inventors have started to try to use graphene for the preparation of the flexible SERS substrate.
Aiming at the technical problems in the prior art, the invention aims to provide a flexible SERS substrate with a graphene/silver nanoflower/PMMA sandwich structure.
The invention further aims to provide a preparation method of the graphene/silver nanoflower/PMMA sandwich structure flexible SERS substrate.
In order to solve the technical problems, the technical scheme of the invention is as follows:
the utility model provides a flexible SERS base of graphite alkene/silver nanometer flower/PMMA "sandwich" structure, includes single-deck graphite alkene, grows in the silver nanometer flower layer of single-deck graphite alkene surface and covers the PMMA film on silver nanometer flower layer surface, makes silver nanometer flower layer centre gripping between single-deck graphite alkene and PMMA film.
Compared with the traditional graphene-precious metal nanostructure SERS substrate and rigid SERS substrate, the graphene/silver nanoflower/PMMA flexible SERS substrate has the advantages that: firstly, silver nanoflowers directly grow on the surface of graphene, so that the silver nanoflowers can be firmly attached to the surface of the graphene; secondly, PMMA (polymethyl methacrylate) has certain strength on one hand and can be used as a support of the flexible SERS substrate; on the other hand, the enhanced SERS substrate has good light transmittance and does not influence the enhancement effect of the SERS substrate; in the third aspect, the silver nanoflowers are firmly fixed between the single-layer graphene and the PMMA film, so that the fastness of the silver nanoflowers in attachment is improved, air is isolated, the silver nanoflowers are effectively prevented from being oxidized, and the service life of the SERS substrate is prolonged. Thirdly, the nano flower-shaped silver can provide a huge SERS effect, and the signal enhancement effect of the nano flower-shaped silver is far better than that of structures such as silver nanoparticles and the like; and fourthly, the single-layer graphene has better flexibility, the PMMA has better flexibility and certain strength, so that the prepared SERS substrate is a flexible substrate, the flexible SERS substrate has wider applicability, and in-situ trace detection can be realized.
The preparation method of the graphene/silver nanoflower/PMMA sandwich structure flexible SERS substrate comprises the following steps: growing a single-layer graphene on a copper foil, growing a layer of silver nanoflowers on the surface of the single-layer graphene by a micro-current assisted chemical reduction method, then covering a layer of PMMA film on the silver nanoflowers, and finally removing the copper foil through corrosion to obtain the nano-silver/copper alloy composite material.
The silver nanoflowers directly grow on the surface of the single-layer graphene, so that the silver nanoflowers can be firmly attached to the surface of the graphene; the silver nanoflower prepared by the micro-current-assisted chemical reduction method has a larger specific surface area and a stronger Raman enhancement effect, and the generated silver nanoflower is embedded with the single-layer graphene, so that the bonding strength between the silver nanoflower and the single-layer graphene is further improved.
Further, the growth method of the single-layer graphene is a CVD (chemical vapor deposition) growth method.
Furthermore, the current of the micro-current assisted chemical reduction method is 50-200 muA/cm-1The growth time is 10-70 s. Embedding graphene-grown copper foil into AgNO3In the solution, a displacement reaction can occur between copper atoms and silver ions to form silver nano islands, which is the first nucleation and growth process of silver nano crystals, in order to form silver nano flowers with tip structures, the second nucleation and growth process of the silver nano crystals is carried out by a micro-current electroplating method, and at the moment, silver nano clusters formed by the silver atoms are directionally attached to the surfaces of the silver nano islands to form the tip structures with excellent SERS effect.
Furthermore, the current is 140 to 180 μ A/cm-1The growth time is 40-60 s.
When the current and the growth time are in the range, the prepared silver nanoflower has a stronger Raman signal enhancement effect.
Furthermore, the electrolyte of the micro-current assisted chemical reduction method is AgNO3The concentration of the electrolyte in the solution is 1.5-2 g/L.
Furthermore, the method for growing the silver nanoflowers by the micro-current assisted chemical reduction method specifically comprises the following steps: the graphene/copper foil composite is used as a negative electrode, the silver foil is used as a positive electrode, and the current is 50-200 mu A/cm-1AgNO with auxiliary electrolysis concentration of 1.5-2 g/L3And reacting the solution with 10-15 g/L of citric acid mixed solution for 10-70 s to obtain the silver nanoflower.
Further, the corrosive liquid used for corroding and removing the copper foil is FeCl3The concentration of the corrosive liquid is 0.5-1M, and the corrosion reaction temperature is 10-20 ℃.
A biosensor comprises the graphene/silver nanoflower/PMMA sandwich structure flexible SERS substrate.
The graphene/silver nanoflower/PMMA sandwich structure flexible SERS substrate is applied to in-situ trace detection of substances.
The beneficial technical effects of the invention are as follows:
(1) the silver nanoflowers directly grow on the surface of the graphene, so that the silver nanoflowers can be firmly attached to the surface of the graphene;
(2) PMMA is used as a support of the flexible SERS substrate, and has good light transmittance;
(3) the nano flower-shaped silver can provide a huge SERS effect, and the signal enhancement effect of the nano flower-shaped silver is far better than that of structures such as silver nanoparticles and the like;
(4) the silver nanoflowers are firmly fixed between the graphene and the PMMA film in a sandwich structure, so that the oxidation of silver can be effectively prevented, and the service life of the substrate is greatly prolonged.
(5) The flexible structure enables the prepared SERS substrate to be attached to surfaces with various shapes for in-situ detection, and in-situ detection of Raman signals is carried out.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
Fig. 1 is a scanning electron microscope image of a precursor base copper foil/graphene/silver nanoflower prepared in example 1;
fig. 2 is a scanning electron microscope image of graphene/silver nanoflower/PMMA prepared in example 1.
In fig. 3, (a) is a schematic detection diagram of the graphene/silver nanoflower/PMMA flexible SERS substrate prepared in example 1; (b) graphene/silver nanoflower/PMMA flexible SERS substrate pair 10 prepared for example 1-12And a Raman enhancement effect graph of M concentration rhodamine 6G (R6G).
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
Term interpretation section:
the flexible substrate is a substrate with small bending rigidity and can be bent randomly along with the deformation of the surface of a jointed object; the rigid substrate has high bending rigidity and cannot be bent arbitrarily along with the deformation of the surface of the attached object.
The copper foil is made of copper and other metals in a certain proportion by forging, and generally comprises 90 foils and 88 foils, namely the copper content is 90% and 88%. The copper foil herein may be either of these two types of copper foils, and the copper foil used in the embodiment is a copper foil having a copper content of 90% available from Joint copper foil (Huizhou) Ltd.
Example 1
1. Growing single-layer graphene by using a CVD (chemical vapor deposition) technology by using a high-purity copper foil as a catalyst, wherein a carbon source is methane, a growth matrix is a copper foil, and the growth conditions are as follows: air pressure of 105Pa, the growth temperature is 1100 ℃, and the growth time is 1 h.
2. A layer of silver nanoflowers grows on the surface of graphene by a micro-current assisted chemical reduction method, and specifically comprises the following steps: graphene/copper foil is used as a negative electrode, silver foil is used as a positive electrode, and the current is 150 muA/cm-1The electrolyte is AgNO with the concentration of 2g/L3The solution and 10g/L citric acid mixture, the reaction time is 50 s.
3. With FeCl at a concentration of 1M3The solution is corrosive liquid, and the copper foil substrate is removed in an environment of 20 ℃.
The scanning electron microscope image of the prepared precursor base copper foil/graphene/silver nanoflower is shown in fig. 1, from which it can be seen that: the diameter of the silver nanoflower is 80-120 nm, the distance between nanoflowers is 50-150 nm, and the length of the branch is 40-60 nm. A scanning electron microscope image of the prepared graphene/silver nanoflower/PMMA is shown in fig. 2, from which it can be seen that: the bottom of the silver nanoflower is in a flake shape, the diameter of the silver nanoflower is 80-120 nm, and the distance between the flakes is 50-150 nm. Detection schematic diagram for preparing graphene/silver nanoflower/PMMA flexible SERS substrate, and flexible SERS substrate pair 10 is adopted-12The M concentration rhodamine 6G (R6G) performs raman enhancement, as shown in fig. 3 (a), where 1 is a silica substrate, 2 is a R6G molecular layer, 3 is a silver nanoflower, 4 is a PMMA thin film, 5 is graphene, the R6G molecular layer 2 is located between the silica substrate 1 and the flexible SERS substrate, laser light is projected from above the flexible SERS substrate, and the obtained enhanced raman scattering signal is detected. Graphene/silver nanoflower/PMMA flexible SERS substrate pair 10-12The Raman enhancement effect of M-concentration rhodamine 6G (R6G) is shown in (b)It can be seen that: as low as 10 for R6G concentration-12M, the detection effect of the flexible SERS substrate is still good, the Raman characteristic peak is clear and visible, and the length of the Raman characteristic peak is 1578cm-1The strongest Raman peak of R6G is located at 614cm, which is the Raman peak of graphene-1The intensity is 2300 counts.
Example 2
1. Growing single-layer graphene by using a CVD (chemical vapor deposition) technology by using a high-purity copper foil as a catalyst, wherein a carbon source is methane, a growth matrix is a copper foil, and the growth conditions are as follows: air pressure of 105Pa, the growth temperature is 1100 ℃, and the growth time is 1 h.
2. A layer of silver nanoflowers grows on the surface of graphene by a micro-current assisted chemical reduction method, and specifically comprises the following steps: graphene/copper foil is used as a negative electrode, silver foil is used as a positive electrode, and the current is 200 mu A/cm-1The electrolyte is AgNO with the concentration of 1.5g/L3The solution and 15g/L citric acid mixture solution, the reaction time is 55 s.
3. With FeCl at a concentration of 0.5M3The solution is corrosive liquid, and the copper foil substrate is removed in the environment of 10 ℃.
Example 3
1. Growing single-layer graphene by using a CVD (chemical vapor deposition) technology by using a high-purity copper foil as a catalyst, wherein a carbon source is methane, a growth matrix is a copper foil, and the growth conditions are as follows: air pressure of 105Pa, the growth temperature is 1100 ℃, and the growth time is 1 h.
2. A layer of silver nanoflowers grows on the surface of graphene by a micro-current assisted chemical reduction method, and specifically comprises the following steps: graphene/copper foil is used as a negative electrode, silver foil is used as a positive electrode, and the current is 50 muA/cm-1The electrolyte is AgNO with the concentration of 1.5g/L3The solution and a 10g/L citric acid mixture, the reaction time is 60 s.
3. With FeCl at a concentration of 0.8M3The solution is corrosive liquid, and the copper foil substrate is removed in an environment of 20 ℃.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (5)
1. A flexible SERS substrate with a graphene/silver nanoflower/PMMA sandwich structure is characterized in that: the composite material comprises single-layer graphene, a silver nanoflower layer growing on the surface of the single-layer graphene and a PMMA film covering the surface of the silver nanoflower layer, so that the silver nanoflower layer is sandwiched between the single-layer graphene and the PMMA film;
the preparation method of the graphene/silver nanoflower/PMMA sandwich structure flexible SERS substrate comprises the following steps: growing a single-layer graphene on a copper foil, growing a layer of silver nanoflowers on the surface of the single-layer graphene by a micro-current assisted chemical reduction method, then covering a layer of PMMA film on the silver nanoflowers, and finally removing the copper foil through corrosion to obtain the nano-silver/copper alloy composite material;
the method for growing the silver nanoflowers by the micro-current assisted chemical reduction method specifically comprises the following steps: the graphene/copper foil composite is used as a negative electrode, the silver foil is used as a positive electrode, the current is 50-200 mu A/cm, and the auxiliary electrolyte is AgNO with the concentration of 1.5-2 g/L3Reacting the solution with a mixed solution of citric acid with the concentration of 10-15 g/L for 10-70 s to obtain a silver nanoflower layer;
the copper foil is removed by corrosion, and the corrosive liquid is FeCl3The concentration of the corrosive liquid is 0.5-1M, and the corrosion reaction temperature is 10-20 ℃.
2. The SERS substrate according to claim 1, wherein: the growth method of the single-layer graphene is a chemical vapor deposition growth method.
3. The SERS substrate according to claim 1, wherein: the current is 140-180 muA/cm, and the growth time is 40-60 s.
4. A biosensor, characterized by: the flexible SERS substrate with the graphene/silver nanoflower/PMMA "sandwich" structure comprises any one of the graphene/silver nanoflower/PMMA "sandwich" structures.
5. The application of the graphene/silver nanoflower/PMMA "sandwich" structure flexible SERS substrate as claimed in any one of claims 1-3 in substance in-situ trace detection.
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| CN110146481B (en) * | 2019-05-07 | 2021-11-09 | 山东师范大学 | Silver nanoflower composite graphene SERS substrate and preparation method and application thereof |
| CN111366571B (en) * | 2020-03-12 | 2021-07-27 | 华东师范大学 | CsPbBr 3-Au-based flexible photoinduced enhanced Raman sensor and preparation and application thereof |
| CN112378893B (en) * | 2020-11-11 | 2023-07-14 | 长春理工大学 | Preparation method of composite SERS substrate for pesticide detection |
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