CN112525883A - Simple SERS enhanced substrate and preparation method and application thereof - Google Patents

Simple SERS enhanced substrate and preparation method and application thereof Download PDF

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CN112525883A
CN112525883A CN202011308352.5A CN202011308352A CN112525883A CN 112525883 A CN112525883 A CN 112525883A CN 202011308352 A CN202011308352 A CN 202011308352A CN 112525883 A CN112525883 A CN 112525883A
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sers
substrate
moo
dye probe
enhanced substrate
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杨艳秋
宋朋
丁勇
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Liaoning University
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Liaoning University
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    • G01—MEASURING; TESTING
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    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • 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

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Abstract

The invention relates to a simple SERS enhanced substrate and a preparation method and application thereof. Synthesis of compound MoO by simple hydrothermal reaction using ammonium molybdate as raw material3By means of SERS technology, different types of dye probe molecules are detected, and the conclusion is that the prepared metal oxide MoO3Can be used as a substrate for SERS enhancement and shows excellent versatility. Most importantly, when MoO3For the substrate, SERS spectra of R6G probe molecules at different excitation wavelengths were compared to infer the dominant SERS enhancement mechanism, revealing the presence of the LSPR effect. In addition, this newly prepared SERS substrate has long-term stability, and the excellent reproducibility of this substrate is determined by the face-scan technique. These findings lay the foundation for the future research on corresponding SERS substrates and mechanisms.

Description

Simple SERS enhanced substrate and preparation method and application thereof
Technical Field
The invention relates to the field of surface enhanced Raman spectroscopy, in particular to a simple SERS enhanced substrate for enhancing SERS effect and a preparation method and application thereof.
Background
Research on the mechanism of Surface Enhanced Raman Scattering (SERS) enhancement has been a hot topic and is the ultimate source of SERS. But it has hitherto been difficult to form a unified explanation due to the diversity and complexity of SERS systems. Many fields of development can be further guided by understanding the SERS mechanism, such as development of SERS nanostructures, etc., so that it is necessary to deepen understanding of the enhancement mechanism of SERS. It is now generally accepted that the physical enhancement electromagnetic field (EM) induced by Local Surface Plasmon Resonance (LSPR) and the chemical enhancement by Charge Transfer (CT) between the substrate and adsorbed molecule are the two most widely accepted mechanisms in SERS.
When the SERS activity and the SERS enhancement factor enhancement mechanism are further determined, the SERS substrate exists densely and indiscriminately, but the reproducibility of the SERS substrate is poor, so that a complex problem occurs, and the technical problems limit researchers to systematically research the enhancement mechanism. In addition, the selection of probe molecules can also participate in the exploration, so that the gap of knowledge is filled, the basic understanding of the scientific researchers on Raman is deepened, and the gap is also important for developing the mechanism based on the Raman analysis technology. At present, the SERS substrate is mainly limited to some precious metals (gold, silver, copper, etc.), but the preparation difficulty is large, the cost is high, the stability and reproducibility are also poor, and the SERS substrate is easy to oxidize and damage, and a great deal of research is devoted to optimizing the SERS substrate, so that how to prepare the SERS enhancing substrate with low cost, uniformity, stability and good reproducibility is explored is still the key of the application and development of the SERS technology, so as to achieve higher enhancement and greater usability.
Disclosure of Invention
The invention aims to provide a simple SERS enhanced substrate which is prepared by a hydrothermal synthesis method and has low cost, good uniformity, good stability and good repeatability.
The invention also aims to use the synthesized simple SERS enhanced substrate in detecting the surface enhanced Raman scattering of the dye probe molecule.
In order to achieve the purpose, the invention adopts the technical scheme that: a simple SERS enhancing substrate which is a compound MoO3。
The preparation method of the simple SERS enhanced substrate comprises the following steps: ammonium molybdate is taken as a raw material, a proper amount of water is added, the mixture is fully and uniformly stirred and then transferred to a reaction kettle, hydrothermal reaction is carried out for 48 hours at 180 ℃, drying is carried out for 24 hours at 60 ℃, and MoO is obtained3。
The simple SERS enhanced substrate provided by the invention is used as a substrate for enhancing the SERS effect in the detection of the enhanced Raman scattering of the molecular surface of the dye probe.
Further, the method is as follows: and dispersing a proper amount of the simple SERS enhanced substrate into the dye probe molecule aqueous solution, stirring the obtained mixture at room temperature for 4 hours, centrifuging to obtain a precipitate, washing with deionized water and ethanol, drying in vacuum to obtain the simple SERS enhanced substrate adsorbed with the dye probe molecules, and uniformly coating the simple SERS enhanced substrate adsorbed with the dye probe molecules on a glass slide for SERS test.
Further, the dye probe molecule is a cationic dye probe molecule or an anionic dye probe molecule.
Further, the cationic dye probe molecule is rhodamine 6G or rhodamine B.
Further, the anionic dye probe molecule is methyl blue.
The invention has the beneficial effects that:
1) in the invention, based on theoretical knowledge, the noble metal, some transition metals and semiconductor nano materials have SERS activity and can generate SERS phenomenon, the transition metal molybdenum is selected, and the product MoO is obtained by using the hydrothermal reaction of metal salt thereof3. SERS characterization is carried out on a series of dye probe molecules to obtain the prepared metal oxide MoO3Can be used as a SERS enhanced substrate and shows excellent long-term stability, repeatability and general performance. Most importantly, when MoO3In the case of a substrate, the existence of the LSPR effect is revealed by comparing SERS spectra of R6G molecules at different excitation wavelengths to infer a main SERS enhancement mechanism. This important finding was the subsequent MoO3The research provides important reference and lays a foundation for the research of related substrates and mechanisms in the future.
2) The invention prepares a novel SERS substrate by a hydrothermal method, and utilizes Energy Dispersion Spectroscopy (EDS) to carry out element analysis, a Scanning Electron Microscope (SEM) to carry out surface appearance analysis, a Transmission Electron Microscope (TEM) to carry out further appearance characterization, and X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) to determine the synthesized specific substance. The experimental result shows that the simple MoO is successfully prepared3A substrate.
3) The invention introduces anion-cation probe molecules with high Raman scattering cross sectionExamine MoO3The substrate enhances the response to the substrate, and the experimental result shows that MoO3The substrate not only responds to common cationic dye molecules rhodamine 6G (R6G) and Rhodamine B (RB), but also has enhanced performance on anionic Raman probe molecules Methyl Blue (MB), and has good performance in the SERS field. In addition, a Raman surface scanning technology is introduced, and experimental results show that the substrate has excellent repeatability.
3) The invention researches MoO at the excitation wavelengths of 532nm and 633nm respectively3The SERS behavior of the R6G probe molecule modified on the substrate shows that the enhancement of the Raman signal observed under 532nm laser irradiation is larger, and meanwhile, the characteristic Raman scattering peaks obtained by the two excitation wavelengths are consistent, namely, the characteristic Raman scattering peaks are expressed as EM effect.
4) The invention is based on the composition MoO3The SERS enhanced substrate can be used as an SERS enhanced substrate to perform SERS detection on a series of dye probe molecules, so that the SERS enhanced substrate has enhanced behaviors on both positive and negative ions, and has excellent universality. In addition to this, the stability over time is known from a second measurement of this sample after a few months. By introducing a surface scanning technology, the substrate has good repeatability, and the SERS substrate with such excellent performance lays a foundation for related substrate research in the future.
5) The invention is based on MoO3The substrate has certain metal property, and further SERS experiments of different wavelengths prove that the EM enhancement is MoO through the reduction of peak intensity and the consistency of peak positions at two wavelengths3The mechanism of (2). The important discovery provides important reference for the deep research of the SERS enhancement mechanism.
6) According to the invention, ammonium molybdate is used as a raw material to generate a hydrothermal reaction in a water system, so that the synthesis of molybdenum oxide is realized, the structure, the morphology and the property of the compound are characterized, and the product is determined. Further, through more comprehensive analysis of different types of anion and cation probe molecules on the substance by means of SERS technology, the result shows that the composition can be used as an SERS substrate to enhance the applied probe molecules, and simultaneously meets the excellent performances of low cost, good stability and the like.
Drawings
FIG. 1 is MoO in example 13EDS map of (a).
FIG. 2 is MoO in example 13SEM image (A) and MoO3TEM image (B) of (A).
FIG. 3 is MoO in example 13XRD pattern of (a).
FIG. 4 is MoO in example 13XPS chart of (a).
FIG. 5 is the MoO prepared in example 13Raman spectrum of the powder (633nm,0.17 mw).
FIG. 6 is MoO3Digital photograph (A in the figure) of (1), MoO to which R6G was adsorbed in a liquid state3Digital photograph (B in the figure) and MoO having R6G adsorbed thereon in solid state3Digital photograph (C in the figure).
FIG. 7 shows MoO having R6G adsorbed thereon in example 23SERS plot of (633nm,0.17 mw).
FIG. 8 shows MoO with RB adsorbed in example 23SERS plot of (633nm,0.17 mw).
FIG. 9 shows MoO with adsorbed MB in example 23SERS plot of (633nm,0.17 mw).
FIG. 10 shows MoO having R6G adsorbed thereon in example 23SERS signal profiles (0.17mw) obtained at 532nm and 633nm excitation wavelengths, respectively.
FIG. 11 is a MoO substrate obtained in example 23Raman signal profiles (633nm,0.17mw) obtained after five months of storage in air.
FIG. 12 is at 606cm-1In the vibration mode, the material has adsorbate R6G (10)-6M) MoO of3Raman scan of (2) (633nm,0.17 mw).
Detailed Description
For better understanding of the technical solution of the present invention, specific examples are described in further detail, but the solution is not limited thereto.
Example 1 a simple SERS enhancement substrate (one) was prepared as follows:
weighing 1g of ammonium molybdate solid, putting the ammonium molybdate solid into a clean beaker, adding 40mL of water, fully and uniformly stirring, transferring the mixture into a reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 48 hours, cooling, and drying the obtained hydrothermal product at 60 ℃ for 24 hours to obtain the simple SERS enhanced substrate.
(II) detection
And respectively carrying out SEM, EDS, TEM, XRD and XPS tests on the obtained simple SERS enhanced substrate.
1. EDS detection is carried out on the prepared simple SERS enhanced substrate, and the result is shown in figure 1. EDS was used for elemental analysis and it was confirmed from fig. 1 that the synthesized material contained Mo and O elements. This study provides the basis for the subsequent determination of specific compositions.
2. SEM and TEM detection is carried out on the prepared simple SERS enhanced substrate, and the result is shown in FIG. 2. As can be seen from FIG. 2, the resulting product has a diameter of 50-100nm and a length of several hundred nanometers. It exists in the form of nanowires and nanorods, the surface of which has a relatively uniform stripe pattern. Characterized by this structure as the following MoO3Experimental exploration of the interaction with the probe molecule provides a certain reference.
3. XRD analysis is carried out on the prepared simple SERS enhanced substrate, and the result is shown in figure 3. As can be seen from fig. 3, the synthesized material was specifically analyzed by XRD. The elements of this composition were identified by EDS analysis as described above but the specific material that had been synthesized could not be identified. However, as can be seen from fig. 3, the main diffraction peaks of the spectrum are accurately labeled as orthogonal moos3(JCPDS 76-1003), the result shows that the simple SERS enhanced substrate synthesized by the method is MoO3。
4. FIG. 4 is a graph further demonstrating that the simple SERS enhanced substrate is MoO based on oxidation state using XPS3And (4) synthesizing. As can be seen from fig. 4, the atomic ratio of O/Mo was found to be 3.2 by correcting the intensities of the O1s and Mo3d peaks by the atomic sensitivity factor. This is very consistent with a nominal value of 3.0. Additionally, annealed MoO3Is occupied by a spin-orbit doublet with peaks at the binding energies 232.38 and 235.53eV, respectively due to MoO3Mo3d of5/2And Mo3d3/2This is related to mo (vi) in the oxidation state. The above results further confirm that the simple SERS enhanced substrate material synthesized by the invention is orthorhombic MoO3。
5. FIG. 5 shows MoO measured at an excitation wavelength of 633nm and a power of 0.17mw3Raman spectrum of the powder, further MoO prepared3Used as a substrate in SERS experiments. As can be seen from the figure, the respective peaks thereof correspond to MoO3Characteristic raman peak of (a). Thus, raman characterization further confirmed that the synthesized material was MoO3And more importantly, provides a reference for subsequent SERS analysis.
Example 2
Application of simple SERS enhanced substrate serving as substrate for enhancing SERS effect in detection of dye probe molecule surface enhanced Raman scattering
The method comprises the following steps:
40mg of MoO prepared in example 1 were taken3Dispersing to 16mL with the concentration of 10-6M in an aqueous solution of R6G, the mixture was stirred at room temperature for 4 hours, centrifuged to take a precipitate, washed repeatedly with deionized water and ethanol, and dried under vacuum to obtain R6G-adsorbed MoO3MoO to which R6G was adsorbed3The coating was uniformly coated on a glass slide and subjected to SERS testing.
40mg of MoO prepared in example 1 were taken3Dispersing to 16mL with the concentration of 10-5M in RB aqueous solution, then stirring the mixture for 4 hours at room temperature, centrifuging to take out precipitate, repeatedly washing with deionized water and ethanol, and drying in vacuum to obtain MoO adsorbed with RB3MoO to which RB is to be adsorbed3The coating was uniformly coated on a glass slide and subjected to SERS testing.
40mg of MoO prepared in example 1 were taken3Dispersing to 16mL with the concentration of 10-5M in MB aqueous solution, stirring the mixture at room temperature for 4 hours, centrifuging to obtain precipitate, repeatedly washing with deionized water and ethanol, and drying under vacuum to obtain MoO adsorbed with MB3MoO to which MB is to be adsorbed3The coating was uniformly coated on a glass slide and subjected to SERS testing.
(II) detection
1. FIG. 6 is MoO3Digital photograph of (A), MoO having R6G adsorbed thereon in liquid state3Digital photograph (B) and MoO having R6G adsorbed thereon in solid state3Digital photo (C). As can be seen from FIG. 6, the successful preparation of MoO in the form of white powder from ammonium molybdate by hydrothermal method3(A) In that respect Then adding a certain amount of MoO3Dispersed in a volume of R6G solution and the mixture was stirred at room temperature for a period of time to see MoO3Can be well dispersed in the solution of R6G to form a uniform and stable solution (B). The precipitate was then centrifuged, washed and dried under vacuum, and finally, MoO having R6G adsorbed in the solid state was obtained3(C) In this state, the surface is clearly seen to be uniform and smooth. The same procedure was followed to obtain solid-state MoO with adsorbed RB and MB3。
2. FIG. 7 examines MoO adsorbing R6G at an excitation wavelength of 633nm and a power of 0.17mw3SERS map of (e). Thus studying the response signal of R6G. R6G probe molecule with high Raman scattering cross section tests MoO3Performance as SERS substrate. The characteristic peaks of R6G can be clearly identified in the figure, where 606 and 770cm-1The peaks at (a) correspond to the in-plane and out-of-plane bending of the C-C-C ring and the C-H in-plane bending vibration, respectively. 1127, 1184, 1361, 1503, 1571 and 1652cm-1Is assigned to a symmetric mode of in-plane C-C tensile vibration. This result indicates MoO3Can be used as a SERS substrate to produce enhancement effect on R6G probe molecules.
3. FIG. 8 is a graph investigating the MoO adsorbing RB at an excitation wavelength of 633nm and a power of 0.17mw3SERS map of (e). As can be seen from the figure, except for the presence of MoO3Besides the characteristic peak of (A), a series of new peaks which belong to the Raman characteristic peak of RB are newly appeared, which indicates that MoO3Can produce enhancement effect on RB probe molecules and is represented as a SERS substrate.
4. FIG. 9 is a graph illustrating the observation of the MoO of MB at an excitation wavelength of 633nm and a power of 0.17mw3SERS map of (e). In addition to the common cationic dye probe molecules,the substrate also has enhanced properties for anionic raman probe molecules, such as MB molecules. As can be seen from the figure, 1180, 1361 and 1617cm are in the MB molecule-1The raman shifts at (a) represent S ═ O symmetric and asymmetric stretching vibrations, C ═ N stretching vibrations. The above results show that MoO3Can be used as a SERS substrate, and has excellent universality by showing SERS enhancement performance on common dye probe molecules such as R6G, RB and MB.
5. FIG. 10 shows MoO having R6G adsorbed thereon3SERS signal profiles obtained at a power of 0.17mw at 532nm and 633nm excitation wavelengths, respectively. Preliminary experiments show that MoO3Is metallic and therefore EM enhancement is presumed to be its most likely SERS mechanism. To confirm this, SERS experiments at different wavelengths were performed. As can be seen from the figure, MoO3The raman signal of R6G was enhanced under both 532 and 633nm laser illumination, indicating that it is SERS-active at both frequencies. However, MoO was observed at 532nm radiation3There is a greater enhancement of the raman signal for R6G, while the characteristic raman scattering signals obtained by the two excitation wavelengths are consistent. Thus, the decrease in peak intensity of R6G and the agreement of the peak positions at the two wavelengths confirm that the EM enhancement is MoO3Has an LSPR effect. Clearly understand MoO3For future MoO3The related research of (2) is of great significance.
6. FIG. 11 shows the substrate MoO at an excitation wavelength of 633nm and a power of 0.17mw3Raman signal profiles obtained after five months of storage in air. The substrate is MoO3Stored under normal atmospheric conditions for five months and then subjected to raman detection again. As can be seen from the figure, MoO3The structure of (a) is still almost unchanged, demonstrating the long-term stability of the newly prepared SERS substrate.
7. FIG. 12 examines the curve at 606cm-1In the vibration mode, the adsorbate R6G (10) is present at a laser wavelength of 633nm and a power of 0.17mw-6M) MoO of3Raman scan of (a). Surface scanning technique for determining SERS substrate MoO modified by R6G3The reproducibility of (2). As can be seen from the figure, each of R6GSERS signal peak is obvious and regular, substrate MoO3Has excellent structural uniformity. SERS surface scanning detection of the R6G molecule is carried out in a certain range, and the excellent repeatability of SERS signals from the substrate/probe system is proved.

Claims (7)

1. The simple SERS enhanced substrate is characterized in that the simple SERS enhanced substrate is a compound MoO3。
2. The preparation method of the simple SERS enhanced substrate is characterized by comprising the following steps: ammonium molybdate is taken as a raw material, a proper amount of water is added, the mixture is fully and uniformly stirred and then transferred to a reaction kettle, hydrothermal reaction is carried out for 48 hours at 180 ℃, drying is carried out for 24 hours at 60 ℃, and MoO is obtained3。
3. The use of the simplified SERS enhancement substrate of claim 1 as a substrate for enhancing SERS effect for detecting surface enhanced raman scattering of dye probe molecules.
4. Use according to claim 3, characterized in that the method is as follows: and dispersing a proper amount of the simple SERS enhanced substrate into the dye probe molecule aqueous solution, stirring the obtained mixture at room temperature for 4 hours, centrifuging to obtain a precipitate, washing with deionized water and ethanol, drying in vacuum to obtain the simple SERS enhanced substrate adsorbed with the dye probe molecules, and uniformly coating the simple SERS enhanced substrate adsorbed with the dye probe molecules on a glass slide for SERS test.
5. Use according to claim 3 or 4, wherein the dye probe molecule is a cationic dye probe molecule or an anionic dye probe molecule.
6. The use according to claim 5, wherein the cationic dye probe molecule is rhodamine 6G or rhodamine B.
7. Use according to claim 5, wherein the anionic dye probe molecule is methyl blue.
CN202011308352.5A 2020-11-20 2020-11-20 Simple SERS enhanced substrate and preparation method and application thereof Pending CN112525883A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105621486A (en) * 2015-12-28 2016-06-01 华东理工大学 SERS (surface enhanced raman scattering) substrate based on plasma semiconductor molybdenum oxide and preparing method thereof
CN110308136A (en) * 2019-06-25 2019-10-08 中国计量大学 A kind of noble metal and MoO3The preparation method and application of self-assembled material
CN110967331A (en) * 2019-12-06 2020-04-07 华东理工大学 Oxidation-reduction-resistant amorphous MoO for SERS substrate3-xPreparation method and application of nanosheet

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105621486A (en) * 2015-12-28 2016-06-01 华东理工大学 SERS (surface enhanced raman scattering) substrate based on plasma semiconductor molybdenum oxide and preparing method thereof
CN110308136A (en) * 2019-06-25 2019-10-08 中国计量大学 A kind of noble metal and MoO3The preparation method and application of self-assembled material
CN110967331A (en) * 2019-12-06 2020-04-07 华东理工大学 Oxidation-reduction-resistant amorphous MoO for SERS substrate3-xPreparation method and application of nanosheet

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
HAO WU等: "Metal oxide semiconductor SERS-active substrates by defect engineering" *
JIAYU MA等: "Facile Fabrication of Amorphous Molybdenum Oxide as a Sensitive and Stable SERS Substrate under Redox Treatment" *

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