CN115184337A - Preparation method of nanoparticle/grating composite SERS substrate - Google Patents
Preparation method of nanoparticle/grating composite SERS substrate Download PDFInfo
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- CN115184337A CN115184337A CN202210902273.XA CN202210902273A CN115184337A CN 115184337 A CN115184337 A CN 115184337A CN 202210902273 A CN202210902273 A CN 202210902273A CN 115184337 A CN115184337 A CN 115184337A
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 55
- 239000000758 substrate Substances 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 title claims abstract description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000010931 gold Substances 0.000 claims abstract description 48
- 229910052737 gold Inorganic materials 0.000 claims abstract description 48
- 239000002245 particle Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000004088 simulation Methods 0.000 claims abstract description 12
- 230000000694 effects Effects 0.000 claims abstract description 10
- 238000010894 electron beam technology Methods 0.000 claims abstract description 7
- 238000005530 etching Methods 0.000 claims abstract description 7
- 230000008033 biological extinction Effects 0.000 claims description 10
- 238000001228 spectrum Methods 0.000 claims description 6
- 230000008878 coupling Effects 0.000 abstract description 4
- 238000010168 coupling process Methods 0.000 abstract description 4
- 238000005859 coupling reaction Methods 0.000 abstract description 4
- 238000004611 spectroscopical analysis Methods 0.000 description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 230000000737 periodic effect Effects 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- XYYVDQWGDNRQDA-UHFFFAOYSA-K trichlorogold;trihydrate;hydrochloride Chemical compound O.O.O.Cl.Cl[Au](Cl)Cl XYYVDQWGDNRQDA-UHFFFAOYSA-K 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 235000012055 fruits and vegetables Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000000447 pesticide residue Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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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- Health & Medical Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to a preparation method of a nanoparticle/grating composite SERS substrate, which solves the problem that the advantages of the composite substrate cannot be exerted to the maximum extent due to the fact that structural factors of the particle/grating composite substrate are not considered in the prior art. The invention exerts the effective coupling between the particles and the grating to obtain the maximum enhancement effect. The invention comprises the following steps: (1) Firstly, carrying out simulation operation of a finite difference time domain method, and designing a grating matched with the nano particles; (2) According to the matching principle of the plasmon resonance peak of the grating and the nanoparticles, the period of the gold grating of the spherical gold nanoparticle array is definitely matched, and the enhancement effect of the substrate is further confirmed through a simulation result; (3) And then preparing the gold grating with the period through electron beam etching, and finally paving the gold nanoparticles on the surface of the grating to obtain the composite SERS substrate.
Description
The technical field is as follows:
the invention belongs to the technical field of trace substance detection, and relates to a preparation method of a nanoparticle/grating composite SERS substrate, wherein the surface enhanced Raman scattering spectroscopy (SERS) substrate can be used for detecting trace substances, such as food additives, pesticide residues in fruits and vegetables and the like.
Background art:
the nanoparticle/grating composite structure is considered to be a novel efficient SERS substrate, and compared with the SERS substrate only composed of particles, the concentration limit of trace substance detection can be further reduced. However, the enhanced performance and structure of such composite substrates are closely related, such as the period of the grating, the size of the nanoparticles, the arrangement, and the like. At present, in the research of the particle/grating composite substrate, no consideration is given to structural factors, and only a certain period of grating and nanoparticles are simply combined together to form the composite SERS substrate, so that the advantages of the composite substrate cannot be exerted to the greatest extent.
The detection limit of a SERS substrate can be improved by a composite structure, such as a combination of nano-metal particles and a nanoscale grating. For example, a double-resonance SERS substrate formed by combining gold particles and a silver grating is prepared by Zhouying and the like, and the enhancement effect of the double-resonance SERS substrate is 10 times that of a single gold particle substrate. (Zhouying, yangjiang, a simple method for preparing a double resonance substrate for SERS detection, optical scattering science, 2014, 26 (1): 23-26). However, the enhancement effect of the dual-resonance substrate can be improved in principle because of the plasmon coupling of the grating and the nanoparticles, and the coupling effect is related to the size and arrangement of the grating structure and the nanoparticles, but the composite SERS substrate manufactured by Zhouying et al does not consider these factors, and singly selects the combination of the silver grating with the period of 350nm and the gold nanoparticles with the average diameter of 25nm, so that the advantages of the composite SERS substrate of the nanoparticles and the grating are not exerted.
The invention content is as follows:
the invention aims to provide a preparation method of a nanoparticle/grating composite SERS substrate, which solves the problem that the advantages of the composite substrate cannot be exerted to the greatest extent due to the fact that structural factors of the particle/grating composite substrate are not considered in the prior art. The invention achieves the maximum enhancement effect by the optimal design of the composite structure and the effective coupling between the particles and the grating.
In order to realize the purpose, the invention adopts the technical scheme that:
a preparation method of a nanoparticle/grating composite SERS substrate is characterized by comprising the following steps: the method comprises the following steps:
(1) Firstly, carrying out simulation operation of a finite difference time domain method, and designing a grating matched with the nano particles;
(2) According to the matching principle of the plasmon resonance peaks of the grating and the nanoparticles, the period of the gold grating of the spherical gold nanoparticle array is determined, and the enhancement effect of the substrate is further confirmed through the simulation result;
(3) And then preparing the periodic gold grating by electron beam etching, and finally paving the gold nanoparticles on the surface of the grating to obtain the composite SERS substrate.
In the step (1), a gold nanoparticle array with the diameter of 25nm and the gap of 2nm is constructed, and the plasma resonance peak position of the gold nanoparticle array is obtained through simulation by a time domain difference method;
in the step (2), the extinction spectrums of the gold gratings with different periods are simulated by a finite time domain difference method, and the period of the grating matched with the gold particle array with the diameter of 25nm and the gap of 2nm is 560nm according to the position of an extinction peak.
In the step (3), the gold grating with the period of 560nm is prepared through electron beam etching, and the width of the grating ridge is 280nm.
Compared with the prior art, the invention has the following advantages and effects:
1. before preparing the particle/grating composite SERS substrate, in order to save time and manufacturing cost, the period and the material of the grating matched with the particle array are confirmed theoretically (through the operation of simulation software), and the combination condition of the nanoparticles and the grating is optimized. On the premise of structural parameters provided by a simulation result, the preparation of the corresponding composite substrate is carried out, the complex of multiple compounding of the grating and the particles with different parameters in an experiment is avoided, and the particles and the grating can be prepared at one time to play the role of the particles and the grating to the maximumAn efficiently coupled composite substrate. Through simulation calculation approach optimization, compared with a single SERS substrate of gold nanoparticles, the prepared composite SERS substrate has the advantages that the enhancement effect is remarkably increased, and the concentration limit can be reduced by two orders of magnitude when R6G molecules are detected. In contrast, they do not consider the matching between the grating and the particles (i.e. a certain particle size and particle spacing, and a grating of a certain material and a certain period is required to match), and therefore they cannot exert the strongest coupling of the electric field between the particles and the grating. Their composite substrate tested a limit concentration of crystal violet of 10 -9 mol/L, the limit concentration of the rhodamine name tested by our composite substrate is 10 -10 mol/L。
2. The composite substrate can detect that the limiting concentration of the R6G solution is 10 -10 mol/L, in contrast to which only 10 can be detected on the gold nanoparticle substrate -8 mol/L。
Description of the drawings:
FIG. 1 is a scanning electron microscope picture of the gold nanoparticle/gold grating composite SERS substrate of the present invention;
fig. 2 shows raman scattering spectra of the gold nanoparticle/gold Grating composite SERS substrate (NPs-scattering) and the R6G solution on the gold nanoparticle SERS Substrate (NPs).
The specific implementation mode is as follows:
in order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not delimit the invention.
The invention relates to a preparation method of a nanoparticle/grating composite SERS substrate, which comprises the steps of firstly carrying out simulation operation of a Finite Difference Time Domain (FDTD) method, designing a grating matched with nanoparticles, theoretically defining a period of a gold grating suitable for a spherical gold nanoparticle array with the diameter of 25nm and the arrangement gap position of 2nm according to the matching principle of plasmon resonance peaks of the grating and the nanoparticles, and further confirming the enhancement effect of the substrate through a simulation result. And then preparing the periodic gold grating by electron beam etching, and finally paving the gold nanoparticles on the surface of the grating to obtain the composite SERS substrate.
The embodiment is as follows:
1. constructing a gold nanoparticle array with the diameter of 25nm and the gap of 2nm, and simulating to obtain the plasma resonance peak position by a time domain difference method: in simulation software, a model with nanoparticles arranged on the surface of a silicon wafer is constructed, the plane of the silicon wafer is an xoy plane, incident light is incident from the negative direction of the z axis, the light wave range is 300-800nm, periodic boundary conditions are set in the directions of the x axis and the y axis, and the boundary condition of a perfect matching layer is set in the direction of the z axis. And (3) arranging a reflection monitor at a position 400nm above the nano particles, arranging a transmission monitor at a position 20nm below the nano particles, and subtracting the sum of the energies of the reflection monitor and the transmission monitor from the incident light to obtain an extinction spectrum of the nano particle array, wherein the wavelength corresponding to the strongest value on an extinction curve is the plasma resonance wavelength.
2. Simulating extinction spectrums of gold gratings with different periods by a finite time domain difference method, and confirming that the grating period matched with the gold particle array is 560nm according to the position of an extinction peak: a model that a gold grating is laid on the surface of a silicon wafer (the grating periods are respectively 520 nm, 540 nm, 560nm, 580 nm and 600 nm) is constructed in simulation software, the plane where the silicon wafer is located is an xoy plane, incident light enters from the negative direction of a z axis, the light wave range is 300-800nm, periodic boundary conditions are set in the directions of the x axis and the y axis, and the boundary condition of a perfect matching layer is set in the direction of the z axis. A reflection monitor is arranged at a position 400nm above the grating, a transmission monitor is arranged at a position 20nm below the grating, the sum of the energies of the reflection monitor and the transmission monitor is subtracted from the incident light to obtain the extinction spectra of the grating with different periods, and the wavelength corresponding to the strongest value on the extinction curve is the plasma resonance wavelength of the grating. The resonant wavelengths of the grating and the nanoparticle array are compared, and the closest grating is the best matching grating.
3. Preparing a gold grating with a period of 560nm by electron beam etching, wherein the width of a grating ridge is 280nm;
4. 150mL of deionized water was added to a 300mL beaker, and 0.01g of trisodium citrate was weighed and dissolved. The solution was then boiled for 15 minutes and 1mL of 25mM tetrachloroauric acid trihydrate solution was added rapidly with vigorous stirring, after 30 seconds the solution turned pale red. Then 3mL of a 25mM tetrachloroauric acid trihydrate solution was added.
5. And standing the reacted solution for 12 hours at room temperature, centrifuging 9mL of the gold nanoparticle solution obtained in the step 4 for 12 minutes at 11000r/min, sucking the supernatant after the centrifugation is finished, adding 8mL of deionized water, performing ultrasonic centrifugation for 5 minutes according to the conditions, and performing ultrasonic dispersion on the centrifuged precipitate by using 1mL of deionized water. Thus obtaining a gold nanoparticle solution with a concentration of 1.64 mg/mL;
6. and (4) taking out 10uL of the gold nanoparticle solution obtained in the step (5), dripping the solution on the surface of the grating, and drying in the air.
The microstructure of the composite substrate prepared by the method is shown in figure 1, wherein the period of the gold grating is 560nm, and gold particles with the diameter of 25nm are distributed at the bottom of the grating groove. The Raman spectrum of the composite substrate and the gold nanoparticle substrate for detecting R6G is shown in figure 2, and the upper curve of figure 2 shows that the limiting concentration of the gold Nanoparticle Substrate (NPs) for detecting R6G solution is 10 -8 mol/L, the curve below the graph in FIG. 2 is that the limiting concentration of R6G solution detected by a particle/Grating composite substrate (NPs-grading) is 10 -10 mol/L。
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all equivalent structural changes made by using the contents of the specification and the drawings of the present invention should be included in the scope of the present invention.
Claims (4)
1. A preparation method of a nanoparticle/grating composite SERS substrate is characterized by comprising the following steps: the method comprises the following steps:
(1) Firstly, carrying out simulation operation of a finite difference time domain method, and designing a grating matched with the nano particles;
(2) According to the matching principle of the plasmon resonance peak of the grating and the nanoparticles, the period of the gold grating of the spherical gold nanoparticle array is determined, and the enhancement effect of the substrate is further confirmed through a simulation result;
(3) And then preparing the gold grating with the period through electron beam etching, and finally paving the gold nanoparticles on the surface of the grating to obtain the composite SERS substrate.
2. The method for preparing the nanoparticle/grating composite SERS substrate as claimed in claim 1, wherein the method comprises the following steps: in the step (1), a gold nanoparticle array with the diameter of 25nm and the gap of 2nm is constructed, and the plasma resonance peak position of the gold nanoparticle array is obtained through simulation by a time-domain difference method.
3. The method for preparing the nanoparticle/grating composite SERS substrate as claimed in claim 1, wherein the method comprises the following steps: in the step (2), the extinction spectra of the gold gratings with different periods are simulated by a finite time domain difference method, and the grating period matched with the gold particle array with the diameter of 25nm and the gap of 2nm is 560nm according to the position of an extinction peak.
4. The method for preparing the nanoparticle/grating composite SERS substrate according to claim 1, wherein the method comprises the following steps: in the step (3), the gold grating with the period of 560nm is prepared by electron beam etching, and the width of the grating ridge is 280nm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103048307A (en) * | 2012-12-23 | 2013-04-17 | 吉林大学 | Enhanced Raman detection substrate based on natural biology super-hydrophobic structure surface and preparation method thereof |
| US20130286467A1 (en) * | 2012-04-26 | 2013-10-31 | Uchicago Argonne, Llc | Multiscale light amplification structures for surface enhanced raman spectroscopy |
| CN213041741U (en) * | 2020-08-12 | 2021-04-23 | 中国人民解放军32181部队 | Anti-polarization sensitive grating-metal nanoparticle sol dual-enhanced substrate |
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- 2022-07-29 CN CN202210902273.XA patent/CN115184337A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130286467A1 (en) * | 2012-04-26 | 2013-10-31 | Uchicago Argonne, Llc | Multiscale light amplification structures for surface enhanced raman spectroscopy |
| CN103048307A (en) * | 2012-12-23 | 2013-04-17 | 吉林大学 | Enhanced Raman detection substrate based on natural biology super-hydrophobic structure surface and preparation method thereof |
| CN213041741U (en) * | 2020-08-12 | 2021-04-23 | 中国人民解放军32181部队 | Anti-polarization sensitive grating-metal nanoparticle sol dual-enhanced substrate |
Non-Patent Citations (2)
| Title |
|---|
| 吴春芳等: "一种光栅/纳米颗粒结构的双共振SERS 基底", 《光学学报》, vol. 42, no. 14, 25 July 2022 (2022-07-25), pages 20 - 25 * |
| 计吉焘;翟雨生;吴志鹏;马祥宇;穆慧惠;王琦龙;: "基于周期性光栅结构的表面等离激元探测", 光学精密工程, no. 03, 15 March 2020 (2020-03-15) * |
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