CN105842227A - Preparation method for surface-enhanced Raman substrate and surface-enhanced Raman substrate structure - Google Patents
Preparation method for surface-enhanced Raman substrate and surface-enhanced Raman substrate structure Download PDFInfo
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- CN105842227A CN105842227A CN201610191504.5A CN201610191504A CN105842227A CN 105842227 A CN105842227 A CN 105842227A CN 201610191504 A CN201610191504 A CN 201610191504A CN 105842227 A CN105842227 A CN 105842227A
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- preparation
- enhanced raman
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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
Abstract
The invention provides a preparation method for a surface-enhanced Raman substrate and a surface-enhanced Raman substrate structure, belonging to the field of preparation of micro-nano structures. The preparation method comprises the following steps: selecting a silicon substrate and etching the silicon substrate to produce a silicon pyramid array; putting the silicon pyramid array into a microwave plasma chemical vapor deposition system for growth of a graphene nanoflake; and coating the surface of the graphene nanoflake with a layer of metal particles so as to obtain the surface-enhanced Raman substrate. The surface-enhanced Raman substrate structure is prepared by using the preparation method. The preparation method in the invention can prepare the uniform surface-enhanced Raman substrate with a large area and ensure the metal particles to be pure and free of contaminations. Meanwhile, the preparation method is simple and convenient, and is low in cost. The surface-enhanced Raman substrate prepared in the invention has strong Raman enhancement characteristics and high sensitivity.
Description
Technical field
The present invention relates to the preparation field of micro nano structure, particularly relate to a kind of surface-enhanced Raman substrate
Preparation method and surface-enhanced Raman substrat structure.
Background technology
Surface enhanced raman spectroscopy (Surface-enhanced Raman Scattering, SERS) is because of permissible
Realize Non-Destructive Testing, fingerprint identification, and there is higher sensitivity and be widely used in chemistry, biology,
Molecular Detection in medicine and other fields and analysis.In recent years, develop on the basis of surface Raman enhancement scatters
The needle point Raman come strengthens scattering technology, and the high sensitivity also having been achieved with single molecules level is explored.Along with micro-
The development of nanofabrication technique, the chip of surface Raman enhancement scattering substrate also achieves commercialization, therefore has
Hope to obtain in many research and detection field and be more widely applied.
In surface enhanced raman spectroscopy, substrate is to determine the vital factor of reinforced effects.The most conventional
Surface enhanced raman spectroscopy substrate mainly include coarse metal surface, metal nanoparticle and polymer thereof with
And there is periodic metal micro-nano structure.In prior art, mostly by chemosynthesis metal nano
The method of grain prepares substrate, and the shape of metallic particles, size and size can be carried out good by such method
Good control.But, there is a lot of drawback in this kind of method, including the chemical reagent in building-up process to metal
The pollution of granule and the aspects such as the large area of substrate and concordance are difficult to ensure that.Further, it is also possible to pass through
Electron beam lithography prepares metal Nano structure substrate, and the Substrate Area that this kind of preparation method prepares is less than normal
And preparation cost is higher.Therefore, need badly at present to develop and a kind of preparation there is stronger Raman trait and high
The method of surface-enhanced Raman substrate of sensitivity.
Summary of the invention
Inventors herein have recognized that, Graphene is as a kind of novel phasmon material, only with himself
Special two-dimension plane structure and excellent electricity, optical property, be expected to serve as a contrast with traditional metal Nano structure
Bear building-up closes has stronger Raman trait and the most highly sensitive surface-enhanced Raman substrate for developing.
Above-mentioned discovery based on inventor, the invention provides the preparation method of a kind of surface-enhanced Raman substrate,
The composite construction with surface-enhanced Raman characteristic is formed, including such as by graphene nanometer sheet and metallic particles
Lower step:
Step 1, choose silicon substrate and perform etching to prepare silicon pyramid array to described silicon substrate；
Step 2, described silicon pyramid array is put in microwave plasma CVD system with life
Long graphene nanometer sheet；
Step 3, at the Surface coating layer of metal granule of described graphene nanometer sheet, it is hereby achieved that institute
State surface-enhanced Raman substrate.
Alternatively, described silicon pyramid array obtains especially by following steps: deposit on described silicon substrate
Silicon nitride film, and described silicon nitride film is carried out photoetching, etching and wet etching, thus obtain institute
State silicon pyramid array.
Alternatively, the condition growing described graphene nanometer sheet is: base vacuum 0.1Pa, methane and hydrogen
Gas flow ratio be 2:1-3:1, air pressure is to keep 1.5-3min under conditions of 500-700Pa.
Alternatively, described silicon pyramid array is micron-scale.
Alternatively, the number of plies of described graphene nanometer sheet is 1～4 layer.
Alternatively, a diameter of 15-80nm of described metallic particles.
Alternatively, the method for coating of described metallic particles be evaporate, sputter, coat in one or more.
Alternatively, described metallic particles is golden or silver-colored.
Present invention also offers a kind of according to the surface-enhanced Raman substrat structure prepared by described preparation method,
Including: silicon pyramid array, it is positioned at the graphene nanometer sheet on described silicon pyramid array surface and is coated on
Metallic particles on described graphene nanometer sheet.
Alternatively, in addition to the tip region of described silicon pyramid array, described graphene nanometer sheet and described silicon
The angle on pyramid surface is not more than 90 °.
The preparation method of the surface-enhanced Raman substrate of the present invention, by sinking in microwave plasma chemical gas phase
Long-pending system grows graphene nanometer sheet, large area and homogeneous surface-enhanced Raman substrate can be prepared,
Additionally, there is no the participation of chemical reagent during the cladding of metallic particles, it is ensured that metallic particles pure with
Avoid being contaminated.Meanwhile, the preparation method of the present invention is simple and convenient, and cost is relatively low.
Surface-enhanced Raman substrate prepared by the present invention, has the strongest Raman and strengthens characteristic and high sensitive
Degree., being shown by test, the Raman signal of the Raman substrate that the present invention obtains has well repetition meanwhile
Property and be prone to location.
According to below in conjunction with the accompanying drawing detailed description to the specific embodiment of the invention, those skilled in the art will
More understand the above-mentioned of the present invention and other purposes, advantage and feature.
Accompanying drawing explanation
Some describing the present invention the most by way of example, and not by way of limitation in detail are concrete
Embodiment.Reference identical in accompanying drawing denotes same or similar parts or part.Art technology
Personnel are it should be understood that what these accompanying drawings were not necessarily drawn to scale.In accompanying drawing:
Fig. 1 is the technological process of the preparation method of surface-enhanced Raman substrate according to an embodiment of the invention
Figure；
Fig. 2 a is the scanning electron microscope side view of the sample after step 1 completes；
Fig. 2 b is the scanning electron microscope side view of the sample after step 2 completes；
Fig. 2 c is the scanning electron microscope side view of the sample after step 3 completes；
Fig. 3 a is that one of them Graphene of the surface-enhanced Raman substrate prepared by the embodiment of the present invention 1 is received
The scanning electron microscope side view in the front of rice sheet；
Fig. 3 b is the scanning electron microscope side view of the reverse side of the graphene nanometer sheet in Fig. 3 a；
Fig. 4 a is that one of them Graphene of the surface-enhanced Raman substrate prepared by the embodiment of the present invention 2 is received
The scanning electron microscope side view in the front of rice sheet；
Fig. 4 b is the scanning electron microscope side view of the reverse side of the graphene nanometer sheet in Fig. 4 a；
Fig. 5 is sieve on the surface-enhanced Raman substrate prepared by embodiments of the invention 2 to variable concentrations
The surface enhanced raman spectroscopy figure of red bright 6G molecular testing；
Fig. 6 is that the same position on the surface-enhanced Raman substrate prepared by embodiments of the invention 2 is to dense
Degree is 1 × 10-13The rhodamine 6G molecule of M carries out the surface enhanced raman spectroscopy figure of 10 tests.
Detailed description of the invention
Fig. 1 is the technique stream of the preparation method of surface-enhanced Raman substrate 4 according to an embodiment of the invention
Cheng Tu.See Fig. 1, the invention provides the preparation method of a kind of surface-enhanced Raman substrate 4, pass through stone
Ink alkene nanometer sheet 2 and metallic particles 3 form the composite construction with surface-enhanced Raman characteristic, including as follows
Step:
Step 1, choose silicon substrate and perform etching to prepare silicon pyramid array 1 to described silicon substrate.
The scanning electron microscope side view of the sample after step 1 completes as shown in Figure 2 a.
Step 2, described silicon pyramid array 1 is put in microwave plasma CVD system with
Growth graphene nanometer sheet 2.The scanning electron microscope side-looking of the sample after step 2 completes as shown in Figure 2 b
Figure.
Step 3, at the Surface coating layer of metal granule 3 of described graphene nanometer sheet 2, such that it is able to obtain
Obtain described surface-enhanced Raman substrate 4.The scanning electron microscopy of the sample after step 3 completes as shown in Figure 2 c
Mirror side view.
The preparation method of the surface-enhanced Raman substrate 4 of the present invention, by microwave plasma chemical gas phase
Depositing system grows graphene nanometer sheet 2, large area and homogeneous surface-enhanced Raman lining can be prepared
The end 4, additionally, do not have the participation of chemical reagent, it is ensured that metallic particles during the cladding of metallic particles 3
3 pure to avoid being contaminated.Meanwhile, the preparation method of the present invention is simple and convenient, and cost is relatively low.
In a preferred embodiment, described silicon pyramid array 1 obtains especially by following steps: in institute
State cvd nitride silicon thin film on silicon substrate, and it is rotten that described silicon nitride film carries out photoetching, etching and wet method
Erosion, thus obtain described silicon pyramid array 1.
In a preferred embodiment, the condition growing described graphene nanometer sheet 2 is: base vacuum 0.1Pa,
Methane is 2:1-3:1 with the gas flow ratio of hydrogen, and air pressure is holding 1.5-3min under conditions of 500-700Pa.
Preferably, described silicon pyramid array 1 is micron-scale.
Seeing Fig. 1, the number of plies of described graphene nanometer sheet 2 is 1～4 layer.
Preferably, a diameter of 15-80nm of described metallic particles 3.
Preferably, the method for coating of described metallic particles 3 be evaporate, sputter, coat in one or more.
Preferably, described metallic particles 3 is golden or silver-colored.Described metallic particles 3 can also be alloy, alloy
Can be gold and the alloy of silver composition.
Present invention also offers a kind of according to the surface-enhanced Raman substrate 4 prepared by described preparation method, bag
Include: silicon pyramid array 1, the graphene nanometer sheet 2 being positioned at described silicon pyramid array 1 surface and bag
Overlay on the metallic particles 3 on described graphene nanometer sheet 2.
Preferably, in addition to the tip region of described silicon pyramid array 1, described graphene nanometer sheet 2 and institute
The angle on the surface stating silicon pyramid array 1 is not more than 90 °.
Surface-enhanced Raman substrate 4 prepared by the present invention, has the strongest Raman and strengthens characteristic and high spirit
Sensitivity., shown by test, the Raman signal tool of the surface-enhanced Raman substrate 4 that the present invention obtains meanwhile
Have the most repeated and be prone to location.
It is described further below in conjunction with more specifically embodiment.
Embodiment 1
Seeing Fig. 1, choose silicon (100) substrate, wherein 100 is the crystal face of silicon, at silicon (100) substrate
The silicon nitride film that upper deposition 60nm is thick, and silicon nitride film is carried out photoetching, etching, wet etching with
Prepare silicon pyramid array 1；Silicon pyramid array 1 is put into microwave plasma CVD
(MPCVD) in system, base vacuum is 0.1Pa, and methane is 2:1 with the gas flow ratio of hydrogen,
Air pressure is holding 3min under conditions of 600Pa, grows graphene nanometer sheet 2；Graphene nano is had in growth
Utilizing the Ag thin film that Deposited By Dc Magnetron Sputtering thickness is 3nm on sheet 2, base vacuum is 5E-9Torr,
Sample stage rotating speed is 10rpm, and sputtering power is 100W, and operating air pressure is 0.004Torr.
Fig. 3 a is one of them Graphene of the surface-enhanced Raman substrate 4 prepared by the embodiment of the present invention 1
The scanning electron microscope side view in the front of nanometer sheet 2；Fig. 3 b is the graphene nanometer sheet 2 in Fig. 3 a
The scanning electron microscope side view of reverse side.It can be seen that graphene nanometer sheet from Fig. 3 a and Fig. 3 b
2 is vertical, and the Ag thin film being coated on graphene nanometer sheet 2 by sputtering is Nanoparticulate, directly
Footpath is about 15nm, and is evenly distributed on the tow sides of graphene nanometer sheet 2.The Graphene of vertical
Nanometer sheet 2 one aspect increases the density of the metallic particles 3 in unit testing volume, is on the other hand also beneficial to
Form the three dimensional structure of metallic particles 3/ graphene nanometer sheet 2/ metallic particles 3, this lining can be effectively improved
The effect of the surface Raman enhancement at the end.
Embodiment 2
Seeing Fig. 1, choose silicon (100) substrate, wherein 100 is the crystal face of silicon, at silicon (100) substrate
The silicon nitride film that upper deposition 60nm is thick, and silicon nitride film is carried out photoetching, etching, wet etching with
Prepare silicon pyramid array 1；Silicon pyramid array 1 is put into microwave plasma CVD
(MPCVD) in system, base vacuum is 0.1Pa, and methane is 3:1 with the gas flow ratio of hydrogen,
Air pressure is holding 3min under conditions of 600Pa, grows graphene nanometer sheet 2；Graphene nano is had in growth
Utilizing the Ag thin film that Deposited By Dc Magnetron Sputtering thickness is 5nm on sheet 2, base vacuum is 5E-9Torr,
Sample stage rotating speed is 10rpm, and sputtering power is 100W, and operating air pressure is 0.004Torr.
Fig. 4 a is one of them Graphene of the surface-enhanced Raman substrate 4 prepared by the embodiment of the present invention 2
The scanning electron microscope side view in the front of nanometer sheet 2；Fig. 4 b is the graphene nanometer sheet 2 in Fig. 4 a
The scanning electron microscope side view of reverse side.It can be seen that graphene nanometer sheet from Fig. 4 a and Fig. 4 b
2 is vertical, and the Ag thin film being coated on graphene nanometer sheet 2 by sputtering is Nanoparticulate, directly
Footpath is about 20nm, and is evenly distributed on the tow sides of graphene nanometer sheet 2.The Graphene of vertical
Nanometer sheet 2 one aspect increases the metallic particles density in unit testing volume, on the other hand forms metal
The three dimensional structure of grain 3/ graphene nanometer sheet 2/ metallic particles 3, the surface that can be effectively improved this substrate is drawn
The effect of graceful enhancing.
Fig. 5 is the variable concentrations of test on the surface-enhanced Raman substrate 4 prepared by the embodiment of the present invention
The surface enhanced raman spectroscopy figure of rhodamine 6G molecule.Four surface enhanced prepared by the present embodiment are drawn
It is 1 × 10 that graceful substrate 4 is separately immersed in concentration-14M、1×10-13M、1×10-12M、1×10-10Sieve of M
Take out in the ethanol solution of red bright 6G molecule and after 1h, after drying up, use Laser Scanning Confocal Microscope Raman spectrometer
Four surface-enhanced Raman substrates 4 are tested.Left inset above Fig. 5 is that surface to be tested increases
Haling the graceful substrate 4 optical imagery in Raman spectrometer, right side illustration is surface-enhanced Raman to be tested
The top view of the scanning electron microscope of substrate 4.From figure 5 it can be seen that the two of rhodamine 6G molecule
Individual principal character peak 613cm-1、755cm-1It is 1 × 10 in concentration-13Can differentiate during M, this reality is described
Execute the surface-enhanced Raman substrate 4 obtained by example and there is the strongest Raman enhancing characteristic and high sensitivity.
Raman spectrometer easily can be found by the optical imagery of pyramid array and demarcate test point
Position, provides the foundation for addressable detection and reperformance test.
Fig. 6 is that the same position on the surface-enhanced Raman substrate 4 prepared by the embodiment of the present invention is to concentration
It is 1 × 10-13The rhodamine 6G molecule of M carries out the surface enhanced raman spectroscopy figure of 10 tests.From Fig. 6
In it can be seen that 10 times test spectral line basically identical, two principal character peaks 613 of rhodamine 6G molecule
cm-1、755cm-1All it is apparent from, illustrates that the Raman signal on this substrate is stablized and favorable repeatability.
So far, although those skilled in the art will appreciate that and the most detailed illustrate and describing the present invention's
Multiple exemplary embodiments, but, without departing from the spirit and scope of the present invention, still can be according to this
Disclosure of invention directly determines or derives other variations or modifications of many meeting the principle of the invention.Cause
This, the scope of the present invention is it is understood that and regard as covering other variations or modifications all these.
Claims (10)
1. a preparation method for surface-enhanced Raman substrate, is formed with metallic particles by graphene nanometer sheet
There is the composite construction of surface-enhanced Raman characteristic, comprise the steps:
Step 1, choose silicon substrate and perform etching to prepare silicon pyramid array to described silicon substrate；
Step 2, described silicon pyramid array is put in microwave plasma CVD system with life
Long graphene nanometer sheet；
Step 3, at the Surface coating layer of metal granule of described graphene nanometer sheet, it is hereby achieved that institute
State surface-enhanced Raman substrate.
Preparation method the most according to claim 1, wherein, described silicon pyramid array is especially by such as
Lower step obtain: cvd nitride silicon thin film on described silicon substrate, and described silicon nitride film is carried out photoetching,
Etching and wet etching, thus obtain described silicon pyramid array.
Preparation method the most according to claim 1 and 2, wherein, grows described graphene nanometer sheet
Condition is: base vacuum 0.1Pa, and methane is 2:1-3:1 with the gas flow ratio of hydrogen, and air pressure is 500-700Pa
Under conditions of keep 1.5-3min.
4. according to the preparation method according to any one of claim 1-3, wherein, described silicon pyramid array
For micron-scale.
5. according to the preparation method according to any one of claim 1-4, wherein, described graphene nanometer sheet
The number of plies be 1～4 layer.
6. according to the preparation method according to any one of claim 1-5, wherein, described metallic particles is straight
Footpath is 15-80nm.
7. according to the preparation method according to any one of claim 1-6, wherein, the bag of described metallic particles
Coating method be evaporate, sputter, coat in one or more.
8. according to the preparation method according to any one of claim 1-7, wherein, described metallic particles is gold
Or silver.
9. a surface-enhanced Raman substrat structure, according to the preparation side according to any one of claim 1-8
Method prepares gained, including: silicon pyramid array, the graphene nano that is positioned at described silicon pyramid array surface
Sheet and be coated on the metallic particles on described graphene nanometer sheet.
Surface-enhanced Raman substrat structure the most according to claim 9, wherein, except described silicon gold word
Outside the tip region of tower array, described graphene nanometer sheet is not more than with the angle on described silicon pyramid surface
90°。
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| CN106248649A (en) * | 2016-08-01 | 2016-12-21 | 中国科学院上海微***与信息技术研究所 | A kind of surface enhanced Raman substrate based on Graphene and preparation method thereof |
| CN106404738A (en) * | 2016-09-05 | 2017-02-15 | 山东师范大学 | Graphene oxide/silver nanoparticle/pyramid-shaped silicon three-dimensional Raman enhanced substrate and preparation method and application thereof |
| CN107119252A (en) * | 2017-05-26 | 2017-09-01 | 云南师范大学 | A kind of silicon substrate surface strengthens the preparation method of Raman substrate |
| CN108226137A (en) * | 2018-01-31 | 2018-06-29 | 山东师范大学 | A kind of flexible, transparent molybdenum disulfide@Argent grains/three-dimensional pyramid structure PMMA SERS substrates preparation method and application |
| CN108411271A (en) * | 2018-05-18 | 2018-08-17 | 杭州电子科技大学信息工程学院 | A method of preparing porous nano steel structure |
| CN108624843A (en) * | 2018-05-18 | 2018-10-09 | 杭州电子科技大学信息工程学院 | A kind of preparation method of surface enhanced Raman scattering substrate |
| CN110745777A (en) * | 2019-10-29 | 2020-02-04 | 江南大学 | Regular pyramid as well as preparation method and application thereof |
| CN113218931A (en) * | 2021-04-25 | 2021-08-06 | 陕西未来健康科技有限公司 | SERS-based liquid cell label-free detection platform and preparation method and application method thereof |
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| CN106248649A (en) * | 2016-08-01 | 2016-12-21 | 中国科学院上海微***与信息技术研究所 | A kind of surface enhanced Raman substrate based on Graphene and preparation method thereof |
| CN106404738A (en) * | 2016-09-05 | 2017-02-15 | 山东师范大学 | Graphene oxide/silver nanoparticle/pyramid-shaped silicon three-dimensional Raman enhanced substrate and preparation method and application thereof |
| CN106404738B (en) * | 2016-09-05 | 2019-12-13 | 山东师范大学 | Graphene oxide/silver nanoparticle/pyramid-shaped silicon three-dimensional Raman enhanced substrate and preparation method and application thereof |
| CN107119252A (en) * | 2017-05-26 | 2017-09-01 | 云南师范大学 | A kind of silicon substrate surface strengthens the preparation method of Raman substrate |
| CN108226137A (en) * | 2018-01-31 | 2018-06-29 | 山东师范大学 | A kind of flexible, transparent molybdenum disulfide@Argent grains/three-dimensional pyramid structure PMMA SERS substrates preparation method and application |
| CN108411271A (en) * | 2018-05-18 | 2018-08-17 | 杭州电子科技大学信息工程学院 | A method of preparing porous nano steel structure |
| CN108624843A (en) * | 2018-05-18 | 2018-10-09 | 杭州电子科技大学信息工程学院 | A kind of preparation method of surface enhanced Raman scattering substrate |
| CN108624843B (en) * | 2018-05-18 | 2020-07-07 | 杭州电子科技大学信息工程学院 | Preparation method of surface-enhanced Raman scattering substrate |
| CN110745777A (en) * | 2019-10-29 | 2020-02-04 | 江南大学 | Regular pyramid as well as preparation method and application thereof |
| CN110745777B (en) * | 2019-10-29 | 2023-04-07 | 江南大学 | Regular pyramid as well as preparation method and application thereof |
| CN113218931A (en) * | 2021-04-25 | 2021-08-06 | 陕西未来健康科技有限公司 | SERS-based liquid cell label-free detection platform and preparation method and application method thereof |
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