CN110658173A - Recyclable flexible surface enhanced Raman substrate and preparation method thereof - Google Patents
Recyclable flexible surface enhanced Raman substrate and preparation method thereof Download PDFInfo
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Abstract
The invention relates to a recyclable flexible surface enhanced Raman substrate and a preparation method thereof, wherein the flexible surface enhanced Raman substrate comprises an organic flexible substrate layer and a metal composite nano material layer formed on the surface of the organic flexible substrate; the metal composite nano material layer comprises at least one of metal nano rods and metal nano wires and at least one of metal nano spheres and metal nano sheets.
Description
Technical Field
The invention relates to a recyclable flexible surface enhanced Raman substrate and a preparation method thereof, belonging to the field of detection devices.
Background
At present, the surface enhanced Raman scattering spectrum is a technical means for detecting trace organic fingerprint molecules, and is widely applied to the fields of food safety, environmental detection, medical detection, chemical and biological analysis and the like. The research, development and preparation of the surface-enhanced Raman substrate are considered as important components in the surface Raman enhancement technology link, and are directly related to the detection sensitivity, repeatability and uniformity of the detection means. At present, the raman enhancement substrate mainly comprises gold, silver and other materials, and the preparation cost is increased because the raw materials are generally noble metals. Meanwhile, the existing raman-enhanced substrate is generally a rigid substrate, lacks advantages in-situ detection and generally cannot be reused. These factors all increase surface enhancementThe popularization difficulty of Raman scattering spectrum detection limits the application range of the Raman scattering spectrum detection. Among the same types of surface enhanced raman substrates, chinese publication No. CN101716839A discloses a large-area metal nanostructure substrate for surface enhanced raman and a method for preparing the same, wherein the surface enhanced raman substrate mentioned above is deposited on a substrate using gold or silver as well. Chinese publication No. CN105372223A discloses Ag/TiO2The flexible and reusable SERS substrate has reusability and the preparation method thereof. Chinese publication No. CN104502323A discloses a transparent flexible surface Raman-enhanced flexible substrate and a preparation method thereof, wherein the method adopts poly-terephthalic acid as a substrate, and the substrate also has flexibility. Chinese publication No. CN105424676A discloses a preparation method and application of a flexible surface-enhanced Raman spectrum substrate, and introduces a preparation process of physically depositing a metal material layer on the surface of an anodic alumina template and also adopting an organic material as a supporting layer to uncover a film. However, these types of surface raman-enhanced substrates are generally prepared by methods with high preparation cost (physical film formation, physical or chemical etching, etc.), and these methods bring expensive preparation cost, and cannot combine high sensitivity, flexibility, in-situ detectability and reusability, which limits practical applications.
Disclosure of Invention
In view of the above problems, the present invention provides a recyclable flexible surface enhanced raman substrate and a method for manufacturing the same.
In one aspect, the invention provides a recyclable flexible surface enhanced raman substrate, which comprises an organic flexible substrate layer and a metal composite nano material layer formed on the surface of the organic flexible substrate layer; the metal composite nano material layer comprises at least one of metal nano rods and metal nano wires and at least one of metal nano spheres and metal nano sheets.
In the present disclosure, a surface enhanced raman substrate includes a metal composite nanomaterial layer and a flexible organic base. The composition of the metal composite nano material layer comprises at least one of metal nano rods and metal nano wires and at least one of metal nano spheres and metal nano sheets. The metal nanowires or/and the metal nanorods form a framework structure with uniform space, and the nanospheres or/and the nanosheets are uniformly embedded in the gaps or the surface positions of the framework structure, so that the sensitivity of the surface enhanced Raman spectrum is improved. That is to say, the composite metal nano structure generates more local state surface plasmon resonance active sites, enhances electromagnetic field coupling and improves the sensitivity of surface enhanced Raman scattering.
Preferably, the material of the organic flexible substrate layer is at least one of polycarbonate, polyurethane, polyacrylic acid and polydimethylsiloxane.
Preferably, the mass content of at least one of the metal nanorods and the metal nanowires in the metal composite nanomaterial layer is not less than 50 wt%; preferably, the mass ratio of the at least one of the metal nanorods and the metal nanowires to the at least one of the metal nanospheres and the metal nanosheets is 3: (0.5 to 3).
Preferably, the diameter of the metal nanospheres is less than 500 nanometers; the diameter of the metal nano sheet is less than 300 nanometers, and the thickness of the metal nano sheet is less than 30 nanometers; the diameter of the metal nano rod is less than 200 nanometers, and the length of the metal nano rod is less than 2 micrometers; the diameter of the metal nanowire is less than 200 nanometers, and the length of the metal nanowire is less than 100 micrometers.
Preferably, the material of the metal composite nano material layer is at least one of platinum, gold, silver and copper; the thickness of the metal composite nano material layer is 0.5-20 microns.
Preferably, the thickness of the organic flexible substrate layer is 1 to 50 mm.
In another aspect, the present invention also provides a method for preparing the flexible surface-enhanced raman substrate, including:
dispersing the metal composite nano material dispersion liquid on the surface of a high molecular polymer mould, and drying to obtain a metal composite nano material layer;
and coating the mixed solution containing the material of the organic flexible substrate layer and the curing agent on the surface of the metal composite nano material layer, and removing the high molecular polymer mould after curing to obtain the flexible surface enhanced Raman substrate.
In the disclosure, the surface-enhanced raman substrate includes a metal composite nanomaterial layer and a flexible organic substrate, wherein the metal composite nanomaterial layer is formed by mixing a plurality of metal nanomaterial dispersions, coating, drying and stripping the surface of the metal nanostructure layer formed by the film formation of the flexible organic substrate, and a flexible surface-enhanced raman spectrum of an embedded structure is formed. Meanwhile, compared with a common adsorption mode, the embedded structure on the surface of the substrate is more stable, and the number of times of recycling is optimized, so that the effect of reducing cost is achieved.
Preferably, a pressure of not more than 10MPa is applied to the obtained flexible surface enhanced Raman substrate and kept for 10 minutes, so that the surface of the flexible surface enhanced Raman substrate is kept flat.
Preferably, the solvent of the metal composite nano-material dispersion liquid is at least one of water, methanol, ethanol, isopropanol and n-butanol.
Preferably, the drying temperature is 75-200 ℃, and the drying time is 5-240 minutes; the curing temperature is 30-150 ℃, and the curing time is 2-12 hours.
Has the advantages that:
on one hand, the preparation method of the recyclable flexible surface enhanced Raman substrate adopts a simple low-energy-consumption wet chemical method to prepare, so that the preparation cost is saved. Secondly, the flexible characteristic of the recyclable flexible surface enhanced Raman substrate determines that the recyclable flexible surface enhanced Raman substrate has great advantages in the field of in-situ surface enhanced Raman detection compared with a rigid substrate. The invention adopts flexible organic matter to solidify and uncover the surface of the formed metal composite nano structure, and aims to provide an embedded, flexible and reusable surface enhanced Raman substrate. The metal composite nano material layer compounded by the metal nano structures with different nano appearances can improve the Raman enhancement effect while keeping the detection uniformity.
Drawings
FIG. 1 is a schematic structural diagram of a recyclable flexible surface enhanced Raman substrate;
FIG. 2 shows the concentration 10-6Adsorbing the methylene blue in mol/L on the surfaces of the samples of the comparative example 1 and the example 1 by using an enhanced Raman spectrum;
FIG. 3 shows the concentration 10-6Adsorbing the methylene blue at mol/L on the surfaces of the samples of the embodiment 1 and the embodiment 2 to enhance the Raman spectrum;
fig. 4 shows that the volume ratio of the silver nanowire and silver nanosphere solution in example 2 is 3:3, detecting effects of the sample on thiram pesticides with different concentrations;
fig. 5 shows that the volume ratio of the silver nanowire and silver nanosphere solution in example 2 is 3:3, detecting effect of the sample on thiram pesticide in the plant radix paeoniae alba;
fig. 6 shows that the volume ratio of the silver nanowire and silver nanosphere solution in example 2 is 3:3 recycling effect of the sample (10 times of repeated use).
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In an embodiment of the present invention, a recyclable flexible surface enhanced raman substrate is shown in fig. 1, and includes a metal composite nanomaterial layer represented by 1, and an organic flexible substrate layer represented by 2. The metal composite nano material layer (surface metal composite structure layer) is attached to the surface of the organic flexible substrate layer in a semi-embedded mode. In an optional embodiment, the material of the metal composite nano material layer is at least one of platinum, gold, silver and copper. In alternative embodiments, the metal composite nanomaterial layer includes at least one of metal nanospheres, metal nanoplates, metal nanorods, metal nanowires, and the like. Wherein the diameter of the metal nanosphere is less than 500 nanometers. The diameter of the metal nano sheet is less than 300 nanometers, and the thickness of the metal nano sheet is less than 30 nanometers. The diameter of the metal nano rod is less than 200 nanometers, and the length of the metal nano rod is less than 2 micrometers. The diameter of the metal nanowire is less than 200 nanometers, and the length of the metal nanowire is less than 100 micrometers. Wherein, the thickness of the metal composite nano material layer can be 0.5 to 20 microns.
In alternative embodiments, the material of the organic flexible substrate layer may be at least one of polycarbonates, polyurethanes, polyacrylics, and polydimethylsiloxanes. Wherein, the thickness of the organic flexible basal layer is 1-50 mm.
In an embodiment of the present invention, the metal composite nano material layer (surface metal structure layer) is formed by mixing a plurality of metal nano material dispersions, coating, drying and forming a film, and curing and uncovering the surface of the metal nano structure layer formed by the flexible organic substrate to form the flexible surface enhanced raman spectroscopy of the embedded structure.
The following exemplarily illustrates a method for preparing a flexible surface enhanced raman spectrum.
A metal composite nanomaterial dispersion (metal nanomaterial dispersion) is prepared. According to the metal composite nano material dispersion liquid with different components, different raw materials are selected to prepare the metal composite nano material dispersion liquid. Specifically, different metal nano material dispersions are mixed, one of nano wires or nano rods is taken as a main body, the mass percent is not less than 50%, one of nano balls or nano plates is taken as an auxiliary body, and the mass percent is not more than 50%. Wherein, the solvent of the metal nanometer material dispersion liquid can be one or a mixture of water, methanol, ethanol, isopropanol and n-butanol. The metal nano material can be nanospheres, nanosheets, nanorods, nanowires and a mixture thereof, and can be prepared by a common chemical method. The material of the metal nano material can be one or combination of platinum, gold, silver and copper.
And coating the metal nano material dispersion liquid on the surface of a high molecular polymer mold, and drying to form a film to obtain the metal composite nano material layer. Specifically, the coating is applied to one surface of a mold with low surface material such as polytetrafluoroethylene, polyvinylidene fluoride or polychlorotrifluoroethylene by one of spin coating, drop coating, bar coating, blade coating and spray coating methods, and dried to form a film. Wherein, the drying temperature can be 75-200 ℃, and the drying time can be 5-240 minutes.
And uniformly coating the solution of the uncured organic flexible substrate layer material on the surface of the dried metal composite nano material layer, curing and uncovering the film to obtain the metal composite nano material. Wherein the curing temperature can be 30-150 ℃, and the curing time can be 2-12 hours.
After stripping, the surface of the flexible surface enhanced Raman substrate is applied with a pressure not exceeding 10MPa and then kept for 10 minutes to ensure the surface is flat.
The preparation method of the recyclable flexible surface enhanced Raman enhancement substrate with the composite nano structure is illustrated by taking a silver nanosphere composite silver nanowire surface metal structure layer and a polydimethylsiloxane organic matter flexible substrate layer as examples. And (3) selecting and mixing ethanol dispersion solutions of the silver nanowires and the silver nanospheres, wherein the mass percentage of the silver nanowire solution is not less than 50%, and the mass percentage of the silver nanospheres is not more than 50%. And spin-coating the mixed dispersion liquid on the surface of a polytetrafluoroethylene die, and drying for 5-240 minutes at the temperature of 75-200 ℃ to form a dry film. And (3) uniformly coating the surface of the dry film with an organic solution mixture of polydimethylsiloxane and a curing agent thereof, and curing for 2-12 hours at the temperature of 30-150 ℃. The composite was peeled off the substrate and held at 10MPa for 10 minutes to ensure surface flatness.
In general, the surface metal composite nano structure is combined with the organic flexible substrate layer in an embedded mode, so that the electromagnetic field coupling of the surface is enhanced, and the sensitivity of surface-enhanced Raman scattering is improved. Meanwhile, compared with a common combination mode, the embedded structure on the surface of the substrate is more stable, the surface structure is more stable, and in-situ detection and recycling are facilitated.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below. In the following examples, the diameter of the silver nanowires in the silver nanowire dispersion is 30 to 60 nm, and the length is 5 to 70 μm.
Example 1
The method for preparing the surface enhanced Raman substrate with the composite nano structure comprises the following steps:
a. selecting an ethanol dispersion of silver nanowires (solid content is 15 mg/ml) and an ethanol dispersion of silver nanospheres (solid content is 15 mg/ml), wherein the average diameter of the silver nanowires is 50 nanometers, the average length of the silver nanowires is 60 micrometers, and the average diameter of the silver nanospheres is 40 nanometers;
b. mixing ethanol solution of silver nanowires and ethanol solution of silver nanospheres in different volume ratios of (1)3:0.5, (2)3:1, (3)3:2 and (4)3:3, and uniformly oscillating;
c. and (c) coating the metal nano material dispersion liquid prepared in the step (b) on a silicon wafer by adopting spin coating, and drying for 60 minutes at the temperature of 120 ℃ to form a metal composite nano material layer (the thickness of each layer is 10 microns).
Example 2:
the method for preparing the recyclable flexible surface enhanced Raman substrate comprises the following steps:
a. selecting an ethanol dispersion of silver nanowires (solid content is 15 mg/ml) and an ethanol dispersion of silver nanospheres (solid content is 15 mg/ml), wherein the average diameter of the silver nanowires is 50 nanometers, the average length of the silver nanowires is 60 micrometers, and the average diameter of the silver nanospheres is 40 nanometers;
b. mixing and uniformly oscillating ethanol solutions of silver nanowires and ethanol solutions of silver nanospheres in different volume ratios of (1)3:0, (2)3:0.5, (3)3:1, (4)3:2 and (5)3: 3;
c. b, coating the metal nano material dispersion liquid prepared in the step b on a polytetrafluoroethylene die by spin coating, and drying for 60 minutes at the temperature of 120 ℃ to form a metal composite nano material layer (the thickness of each layer is 10 microns);
d. uniformly coating the surface of the dry film with an organic solution mixture of polydimethylsiloxane and a curing agent thereof, and curing for 12 hours at the temperature of 75 ℃;
e. after the solidification is finished, the polytetrafluoroethylene mold is removed, and a flexible metal nano material embedded high-molecular polymer structure is obtained, wherein the thickness of the organic flexible substrate layer is 10 mm;
f. after stripping, the composite structure is applied with a pressure of 10MPa for 10 minutes to ensure the surface to be flat, and the final flexible surface enhanced Raman substrate is obtained.
Comparative example 1:
a. selecting an ethanol dispersion (solid content 15 mg/ml) of silver nanowires, wherein the silver nanowires have an average diameter of 50 nm and an average length of 60 microns;
b. and (b) taking the metal nano material dispersion liquid prepared in the step (a), coating the metal nano material dispersion liquid on a silicon chip by adopting spin coating, and drying the silicon chip for 60 minutes at the temperature of 120 ℃ to form a dry film.
The surface enhanced substrates prepared in comparative example 1, example 1 and example 2 were all prepared to a size of 0.5cm by 0.5cm and were ready for raman spectroscopy testing. The detection indicator is selected from methylene blue, thiram and malachite green. A micro laser raman system (inVia, Renishaw, UK) equipped with a 50-fold objective lens was used to collect raman spectra. While employing a laser wavelength of 633 nm as the incident wavelength.
Comparative example 1, using 10-6In the case where 50. mu.L of methylene blue in mol/L was dropped on the surface of the substrate, and the silicon wafer was used as the base, it can be seen from FIG. 2 that the intensity of the Raman spectrum was increased as the ratio of the silver nanoparticles in the whole system was increased. Therefore, it was confirmed that the silver nanowire composite silver nanoparticle structure is superior to the single silver nanowire structure.
Comparative example 1, example 2, using 10-6As can be observed by comparing FIG. 2 with FIG. 3, the intensity of the Raman spectrum of the surface enhanced Raman substrate sample using PDMS as the base in example 2 is significantly stronger than that of the sample using the silicon wafer as the base in example 1. Therefore, the surface enhanced Raman effect of the polydimethylsiloxane as the flexible substrate can be determinedA surface enhanced Raman substrate better than a silicon wafer substrate.
Meanwhile, the sample with the best effect in example 2, namely the sample prepared by the volume ratio of the silver nanowire ethanol solution to the silver nanosphere ethanol solution of 3:3, is selected for detecting thiram which is a harmful substance to human bodies and the environment, and fig. 4 shows that different concentrations (10% of ethanol) are detected-10～10-5mol/L) the detection effect of thiram, and the enhancement factor of the Raman signal reaches 2.5 multiplied by 107. The results prove that the flexible Raman enhancement substrate made of the composite nano material can obviously improve the sensitivity of surface enhanced Raman detection.
In the aspect of in-situ test, the sample prepared by the volume ratio of the silver nanowire ethanol solution to the silver nanosphere ethanol solution of 3:3 is subjected to in-situ pesticide detection on the surface of plant spatholobus suberectus leaf, as shown in fig. 5, the flexible substrate can be proved to be directly wiped to detect that 10 mu L of the pesticide is dripped on the surface of the plant spatholobus suberectus leaf, and the concentration of the pesticide is 10 mu L-4The pesticide thiram on the surface of the plant leaf is mol/L.
It is noted that when the sample prepared by using the silver nanowire and silver nanosphere solution in the volume ratio of 3:3 is used for detecting the pesticide thiram, the sample is also subjected to a flushable recycling experiment, and the recycling mode is tested by detecting, flushing with deionized water and dripping again the indicator, as shown in fig. 6, and the sample still maintains 54.7% of performance after 10 cycles.
Therefore, the sample prepared by the volume ratio of the silver nanowire ethanol solution to the silver nanosphere ethanol solution of 3:3 in the embodiment 2 has the best surface-enhanced raman effect. The structure has the advantages of low preparation cost, high detection sensitivity, in-situ detection, recycling, economic and practical values, and wide application in the fields of food safety, environmental detection, medical detection, chemical and biological analysis and the like.
It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to preferred versions, it will be understood by those skilled in the art that various changes in form and techniques may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (10)
1. A recyclable flexible surface enhanced Raman substrate is characterized by comprising an organic flexible substrate layer and a metal composite nano material layer formed on the surface of the organic flexible substrate layer; the metal composite nano material layer comprises at least one of metal nano rods and metal nano wires and at least one of metal nano spheres and metal nano sheets.
2. The flexible surface-enhanced raman substrate according to claim 1, wherein the material of said organic flexible substrate layer is at least one of polycarbonate, polyurethane, polyacrylic, and polydimethylsiloxane.
3. The flexible surface-enhanced raman substrate according to claim 1 or 2, characterized in that a mass content of at least one of metal nanorods and metal nanowires in said metal composite nanomaterial layer is not less than 50 wt%; preferably, the mass ratio of the at least one of the metal nanorods and the metal nanowires to the at least one of the metal nanospheres and the metal nanosheets is 3: (0.5 to 3).
4. A flexible surface enhanced raman substrate according to any one of claims 1 to 3, characterized in that said metal nanospheres have a diameter of less than 500 nanometers; the diameter of the metal nano sheet is less than 300 nanometers, and the thickness of the metal nano sheet is less than 30 nanometers; the diameter of the metal nano rod is less than 200 nanometers, and the length of the metal nano rod is less than 2 micrometers; the diameter of the metal nanowire is less than 200 nanometers, and the length of the metal nanowire is less than 100 micrometers.
5. The flexible surface-enhanced Raman substrate of any one of claims 1-4, wherein the material of the metal composite nanomaterial layer is at least one of platinum, gold, silver, and copper; the thickness of the metal composite nano material layer is 0.5-20 microns.
6. The flexible surface-enhanced Raman substrate of any one of claims 1-5 wherein the organic flexible base layer has a thickness of 1 to 50 millimeters.
7. A method of making a flexible surface-enhanced Raman substrate according to any one of claims 1-6, comprising:
dispersing the metal composite nano material dispersion liquid on the surface of a high molecular polymer mould, and drying to obtain a metal composite nano material layer;
and coating the mixed solution containing the material of the organic flexible substrate layer and the curing agent on the surface of the metal composite nano material layer, and removing the high molecular polymer mould after curing to obtain the flexible surface enhanced Raman substrate.
8. The flexible manufacturing method according to claim 7, wherein the surface of the flexible surface-enhanced Raman substrate is kept flat by applying a pressure of not more than 10MPa to the flexible surface-enhanced Raman substrate for 10 minutes.
9. The method according to claim 7 or 8, wherein the solvent of the metal composite nanomaterial dispersion is at least one of water, methanol, ethanol, isopropanol, and n-butanol.
10. The method according to any one of claims 7 to 9, wherein the drying is carried out at a temperature of 75 to 200 ℃ for 5 to 240 minutes; the curing temperature is 30-150 ℃, and the curing time is 2-12 hours.
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Cited By (1)
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| CN112697771A (en) * | 2020-12-14 | 2021-04-23 | 广西民族大学 | Method for detecting formaldehyde in food by using surface enhanced Raman spectroscopy based on gold nanorod substrate |
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| US20120300203A1 (en) * | 2011-05-27 | 2012-11-29 | Som Tyagi | Flexible sers substrates with filtering capabilities |
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