CN108226079B - Metallic graphite carbon alkene multilayer resonance structure enhances the infrared double spectra devices of Raman and preparation method - Google Patents
Metallic graphite carbon alkene multilayer resonance structure enhances the infrared double spectra devices of Raman and preparation method Download PDFInfo
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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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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
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Abstract
A kind of metallic graphite carbon alkene multilayer resonance structure enhancing infrared double spectra devices of Raman, including substrate, metallic reflector, dielectric layer, metal micro antenna, graphene film, metal nanoparticle.Dielectric layer forms metal-dielectric-metal reflection-type micron antenna structure between metal micro antenna and metallic reflector.Graphene film forms nano gap between metal nanoparticle and metal micro antenna.Under infrared waves irradiation, the antenna resonance effect of metal micro antenna is excited, enhances the infrared absorption spectrum signal of trace molecules within the scope of broadband.Under visible light wave range laser irradiation, the local surface phasmon of metal nanoparticle is excited, the nano gap between metal nanoparticle and metal micro antenna generates high-intensitive local electric field mode of resonance, enhances the Raman scattering signal of trace molecules.The present invention has enhancing wide waveband, and enhancement factor is high, can large area processing, low in cost, the advantages that detecting material category is wide.
Description
Technical field
The present invention relates to Surface-enhanced spectroscopic technical fields, more particularly to one kind, and surface Raman light is realized on individual devices
Spectrum and the device and preparation method thereof of the double enhancings of surface infrared absorption spectrum.
Background technique
Surface Enhanced spectral technique is a kind of molecular spectrum detection skill to be grown up based on surface phasmon effect
Art is the powerful tools of the important informations such as determining biomolecule composition and structure, in food safety, environmental monitoring, chemical analysis
It has broad application prospects with fields such as biologic medicals.It is Surface Enhanced Raman Scattering Spectrum that the technology is most representational
Technology (Surface-enhanced Raman scattering, SERS) and surface-enhanced infrared spectroscopy technology
(Surface-enhanced infrared absorption, SEIRA).Wherein, SERS technology can be with chemical in molecular detection
Polarizability change information caused by key chattering, and SEIRA technology can be become with dipole moment caused by chemical bond oscillations in molecular detection
Change information.Thus, they are two kinds of complementary molecular engineerings, and any single technology (SERS or SEIRA) is only capable of molecular detection
Partial vibration mode, the polarizability and dipole moment change information of molecule can not be obtained simultaneously.In order to which chemistry can be obtained comprehensively
The advantage of both technologies is combined, is proposed by the structural information of the numerous biomolecule of key chattering mode, researcher
Surface Raman and the double enhancing technologies of infrared spectroscopy, realize the detection to molecular polarizability and dipole moment on the same base.At present
There are two types of resolving ideas.
First is that preparing metal nanoparticle, local EMR electromagnetic resonance mode is generated in visible and infrared two wave bands.Naomi
J.Halas etc. obtains the double enhancing signals of SERS and SEIRA spectrum using gold nano-spherical shell array of structures for the first time.It is received to improve
The pattern of rice grain, Wen-Bin Cai etc. are prepared for nano grain of silver sub-island film, and realize the SEIRA and SERS to ferroheme
Spectral detection.Monica Baia etc. has obtained self-assembling of gold nanoparticles using successive sedimentation method, realizes p-aminophenyl thiophenol
SERS the and SEIRA spectral signal of molecule detects.Jiannian Yao etc. assembles netted gold nano grain, to tested molecule
SERS enhancement factor is 106, SEIRA enhancement factor is 102.Although such method be successfully realized on the same chip SERS with
The double enhancings of SEIRA spectrum, but the reinforcing effect of infrared band SEIRA is poor, enhancement factor is only 102。
Second is that design metal nano antenna, generates local EMR electromagnetic resonance mode in visible and infrared two wave bands.2013,
Cristiano D ' Andrea etc. devises gold nano antenna structure array using electron beam lithography, by changing exciting field
Polarization direction infrared band excitation antenna antenna resonance effect, to generate high-intensitive sharp local EMR electromagnetic resonance
Peak.This method has increased substantially 6 × 10 to the SEIRA enhancement factor of methylene cyan molecule5.However, being completed in device fabrication
Afterwards, resonance frequency immobilizes.Narrow spectrum enhancing wave band can not cover in infrared signature fingerprint region so that the device is only
SEIRA spectral detection can be carried out to a few molecules.Meanwhile the SERS enhancement factor of the substrate only has 102。
In conclusion although both the above method has been able to achieve Raman signal and infrared absorption spectrum to test substance
Double reinforcing effects of signal, still, they are all that enhancement factor is cost to sacrifice one of them (SERS or SEIRA), nothing
Method guarantees that Raman signal and infrared spectroscopy signals all have high enhancement factor.
Summary of the invention
The present invention for overcome the deficiencies in the prior art, proposes a kind of based on the enhancing drawing of metallic graphite carbon alkene multilayer resonance structure
Graceful infrared double spectra devices and preparation method excite metal nano by metal nanoparticle in conjunction with metal micro antenna respectively
Particle visible light wave range local plasmon bulk effect and metal micro antenna infrared band antenna resonance effect, thus
It realizes double reinforcing effects of test substance Raman spectrum and infrared absorption spectrum, there is easy to use, enhancement factor height, it can big face
Product processing, realizes the advantages that a variety of one steps of unknown molecular detect, can be used for the fields such as environmental monitoring, food safety.
To solve technical problem of the invention, used technical solution are as follows:
Enhance the infrared double spectra devices of Raman based on metallic graphite carbon alkene multilayer resonance structure, including sets gradually from bottom to top
Substrate, metallic reflector, dielectric layer, metal micro antenna, graphene film and metal nanoparticle.
The dielectric layer forms metal-dielectric-metal reflection between metal micro antenna and the metallic reflector
Type micron antenna structure, in the SEIRA performance of infrared band enhancing device.
The graphene film is formed between nanometer between the metal nanoparticle and the metal micro antenna
Gap, in the SERS performance of visible light wave range enhancing device.
The metal micro antenna is the micron aerial array by designing different zones on the dielectric layer, each
Region corresponds to a kind of micron antenna of specific dimensions, so that micron antenna has a specific resonance peak (corresponding resonance wavelength
For λ).By design multiple parameters incremental variations micron aerial array region (such as: region 1, region 2 ... ..., region 10,
Correspond respectively to resonance wavelength1, λ2... ..., λ10) resonance peak of Lai Shixian antenna is distributed in 3~16 μm of infra-red ranges, it can
To generate antenna resonance effect in the case where infrared waves excite, to generate strong local electric field at metal micro antenna edge.When
When antenna resonant frequency is consistent with the molecular vibrational frequency of substance to be detected, it can greatly enhance tested surrounding molecules unit space
Interior electromagnetic field intensity visits the Selective long-range DEPT and broadband of testing molecule difference vibration mode to realize in different zones
It surveys.The areal is 2~10, and the areal extent in each region is in 200 μm * 200 μm~1mm*1mm；Each region
In micron aerial array figure it is the same, dimension of picture and cycle parameter are different, can be according to the parameter designing of claim.
The metal nano, which visits particle, can generate local surface phasmon under visible light wave excitation, thus in metal
Strong local electric field is generated around nano particle, further makes metal nanoparticle and metal micro using graphene nano gap
Antenna couples, and improves the SERS performance of device.
This double enhancing device is by separately detecting the infra-red absorbance signals and Raman scattering signal of test substance, to determinand
The molecular structure of matter carries out comprehensive accurate Analysis.
Further, the metal micro antenna in the transverse direction of device in rectangle, square, circle, ellipse,
Hexagon or crux.The size and periodic regime of metal micro antenna are 1 μm~10 μm, and thickness range is 20~200nm.
Further, the graphene film is 1~10 layer, and thickness is less than 5nm.
Further, the metal nanoparticle particle size range is 10~300nm, and metal material is selected from gold, silver, copper, aluminium.
Further, it is 20~1000nm that the dielectric layer, which is thickness range, is located at metal micro antenna and metallic reflection
Reflection-type micron antenna structure is formed between layer.The material of dielectric layer is infrared-transparent material, be can be selected from: Al2O3, KBr, MgF2,
CaF2, BaF2, AgCl, ZnSe, SiO2, diamond-like carbon film.
Present invention further propose that enhancing the preparation method of the infrared double spectra devices of Raman above.The following steps are included:
(1) it prepares metallic reflector: sinking to the bottom one layer of metal layer of upper deposition using magnetron sputtering or electron beam evaporation methods,
As reflecting layer.
(2) preparation media layer: using the method for electron beam evaporation plating, atomic deposition or molecular beam epitaxial growth in metallic reflection
Metallization medium layer on layer.
(3) metal micro antenna is prepared: using photoetching techniques such as ultraviolet photolithographic, laser direct-writings, in conjunction with electron beam evaporation plating, magnetic
The methods of control sputtering, hot evaporation the deposited metal micron antenna on dielectric layer.
(4) it shifts graphene film: utilizing mechanical stripping technique or process for preparing graphenes by chemical vapour deposition film, and
The graphene being prepared is transferred on metal micro antenna.The number of plies of graphene film is 1~10 layer, and multilayered structure can be with
It is realized by directly growing multi-layer graphene or multiple branch mode.
(5) metal nanoparticle is prepared: using the methods of electron beam evaporation plating, magnetron sputtering, hot evaporation in graphene film
Upper depositing metallic nanoparticles.Further, the metal nanoparticle can pass through electron beam evaporation plating, magnetron sputtering, hot evaporation
With slow rateDeposition directly obtains, and the sheet metal thickness ranges of deposition are 3~20nm；Can also further it pass through
High temperature (300~500 DEG C) annealing way controls the size of metal nanoparticle, and particle size range is in 10~300nm；Metal material choosing
From gold, silver, copper, aluminium.
Compared with the existing technology, the present invention has the advantage that
First, double enhancing devices of the invention use processing method from bottom to top, and metal micro antenna and metal
The preparation method of nano particle is mutually compatible with standard microlithographic technique and coating process, have processing technology it is simple, can batch
The clear superiority that metaplasia produces.
Second, the present invention can be by accurately controlling the size and cycle parameter of metal micro antenna, in infrared band pair
Its resonant wavelength is accurately controlled, while being imitated using the reflection-type micron antenna structure method amber resonance that reflecting surface is formed up and down
It answers, further enhances the local to infrared waves, to realize the maximum reinforcing effect to test substance infrared spectroscopy signals；Together
When, by designing the metal micro antenna of different sizes and cycle parameter in the different zones of same substrate, keep its generation humorous
Vibration mode, so that realizing enhances detection to the broadband of test substance.
Third, graphene is as a kind of two-dimensional material, and thickness only has 0.34nm, and the present invention is using graphene as sub-nanometer
Interlayer is clipped between metal nanoparticle and metal micro antenna, is formed nano gap, is made metal nanoparticle not only in level
With the Mode Coupling between nano particle on direction, while there is metal nanoparticle and metal micro day in vertical direction
Coupling between line, so as to greatly enhance the SERS performance of device.Meanwhile π-π between graphene and molecule stack and
Chemical enhancement caused by electric charge transfer also has certain facilitation to SERS.
4th, the present invention realizes the measurement of trace molecules Raman spectrum and infrared spectroscopy signals in same device simultaneously,
The step of remaking device and sample is also needed when avoiding replacement measurement method, can be realized the complete of trace molecules vibration information
Whole measurement accelerates sample detection speed, improves work efficiency.
As it can be seen that the present invention can be achieved at the same time the dual humidification of Surface Raman Spectra and surface infrared spectrum, and have
Have high sensitivity, stability is good, can large area processing, broadband enhancing detection the advantages that, be with a wide range of applications.
Detailed description of the invention
Fig. 1 is that metallic graphite carbon alkene multilayer resonance structure enhances the infrared double spectra device schematic diagrames of Raman；
Fig. 2 is the schematic diagram on same device including multiple and different regions；
Fig. 3 (a)-Fig. 3 (f) is rectangle, square, disc, ellipse, hexagon, the metal micro day of crux
Line schematic diagram；
The schematic three dimensional views of metal micro antenna when Fig. 3 (g) is square for section；
Fig. 4 is the preparation flow figure that metallic graphite carbon alkene multilayer resonance structure enhances the infrared double spectrographic techniques of Raman and device；
Fig. 5 (a) is micron rectangle golden light grid/aluminium oxide/gold reflecting layer reflection-type micron antenna structure SEM picture；
Fig. 5 (b) is the SEM picture that graphene and silver nano-grain cover back reflection type micron antenna structure；
Fig. 6 (a) is the grain size distribution of silver nano-grain；
Fig. 6 (b) is the ultraviolet-visible absorption spectroscopy of silver nanoparticles with different particle diameters；
Fig. 7 (a) is the Raman spectrum of double enhancing devices after silver nanoparticles with different particle diameters；
Fig. 7 (b) is the average Raman spectrum of the rhodamine R6G solution of different molecular concentration；
Fig. 8 (a) is the reflectance spectrum of double enhancing devices under the conditions of different grating line widths；
The reflectance spectrum of Fig. 8 (b) double enhancing devices under the conditions of different grating line widths after being spin coating ethylene oxide PEO；
Fig. 8 (c) is the enhancing vibration signal curve of PEO molecule after Baseline Survey.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawing to of the invention
Preferred embodiment is described in further detail.Identical appended drawing reference represents same or similar component in attached drawing.
Referring to Fig. 1, the metallic graphite carbon alkene multilayer resonance structure enhancing infrared double spectra devices of Raman that the present invention designs include
Substrate 1, metallic reflector 2, dielectric layer 3, metal micro antenna 4, graphene film 5 and the metal set gradually from bottom to top
Nano particle 6.When test, detection substance 7 to be measured is placed on device by modes such as spraying, spin coatings.It is micro- that dielectric layer 3 is located at metal
Between rice antenna 4 and metallic reflector 2, metal-dielectric-metal reflection-type micron antenna structure, the thickness model of dielectric layer 3 are formed
It encloses are as follows: the material of 20~1000nm, dielectric layer are infrared-transparent material, be can be selected from: Al2O3, KBr, MgF2, CaF2, BaF2,
AgCl, ZnSe, SiO2, diamond-like carbon film.The number of plies of graphene film 5 is 1~10 layer, is located at the metal nanoparticle 6
Between the metal micro antenna 4, nano gap is formed, metal nanoparticle is coupled with metal micro antenna, mentions
The SERS performance of high device.The particle size range of metal nanoparticle 6 is 10~300nm, and metal material is selected from gold, silver, copper, aluminium.
In the above structure, metal micro antenna 4 can generate antenna resonance effect under infrared waves excitation, thus in gold
Belong to 4 edge of micron antenna and generates strong local electric field.Further by dielectric layer 3 different zones design different structure it is micro-
Rice aerial array, so that the resonance peak of metal micro antenna 4 is distributed in 3~16 μm of infra-red ranges.When antenna resonant frequency with
When the molecular vibrational frequency of substance 7 to be detected is consistent, it can greatly enhance the electromagnetic field intensity in tested surrounding molecules unit space
Degree detects the Selective long-range DEPT and broadband of testing molecule difference vibration mode to realize in different zones.Metal nano
Local surface phasmon can be generated under visible light wave excitation by visiting particle 6, to generate around metal nanoparticle 6 strong
Local electric field further couples metal nanoparticle 6 with metal micro antenna 4 using graphene nano gap, mentions
The SERS performance of high device.It, can be to be measured by separately detecting the infrared vibration signal and Raman scattering signal of test substance 7
The molecular structure of substance 7 carries out comprehensive accurate Analysis.
Referring to fig. 2, the areal is 2~10, and the areal extent in each region is in 200 μm * 200 μm~1mm*
Between 1mm；Micron aerial array figure in each region is the same, and structure size and cycle parameter are different.Each region
The micron antenna of corresponding a kind of specific dimensions, so that micron antenna has a specific resonance peak (corresponding resonance wavelength is λ).
By the micron aerial array region for designing multiple parameters incremental variations.Such as: region 1, region 2 ... ..., region 10, respectively
Corresponding to resonance wavelength1, λ2... ..., λ10.To realize that the resonance peak of antenna is distributed in 3~16 μm of infra-red ranges.
The shape of metal micro antenna 4 selects according to actual needs, can be rectangle, square, circle, ellipse, six
One or more kinds of combinations of side shape, crux etc..Wherein Fig. 3 (a)~Fig. 3 (f) is metal micro antenna in double boosters
Sectional view in the transverse direction of part, Fig. 3 (g) give the schematic three dimensional views for the micron antenna structure that section is square.Gold
The size and periodic regime for belonging to micron antenna are 1 μm~10 μm, and thickness range is 20~200nm.
Fig. 4 is the flow chart for preparing the metallic graphite carbon alkene multilayer resonance structure enhancing infrared double spectra devices of Raman:
Step S1: metallic reflector is prepared.One layer of gold is deposited on substrate 1 using magnetron sputtering or electron beam evaporation methods
Belong to layer, as metallic reflector 2.
Step S2: preparation media layer.Using the method for electron beam evaporation plating, atomic deposition or molecular beam epitaxial growth in metal
Metallization medium layer 3 on reflecting layer 2.
Step S3: metal micro antenna is prepared.Using microlithography technologies such as ultraviolet photolithographic, laser direct-writings, in conjunction with electron beam
The methods of vapor deposition, magnetron sputtering, hot evaporation deposited metal micron antenna 4 on dielectric layer.The shape of metal micro antenna 4 can be with
Select the one or more of them combination of rectangle, square, circle, ellipse, hexagon, crux etc., metal micro day
The size and periodic regime of line are 1 μm~10 μm, and thickness range is 20~200nm.
Step S4: transfer graphene film.It is thin using mechanical stripping technique or process for preparing graphenes by chemical vapour deposition
Film 5, and the graphene being prepared is transferred on metal micro antenna 4；The number of plies of graphene film 5 is 1~10 layer, multilayer
Structure can be realized by directly growing multi-layer graphene or multiple branch mode；
Step S5: metal nanoparticle is prepared.Using the methods of electron beam evaporation plating, magnetron sputtering, hot evaporation in graphene
Depositing metallic nanoparticles 6 on film 5.Metal nanoparticle 6 can be by electron beam evaporation plating, magnetron sputtering, hot evaporation with slow
RateDeposition directly obtains, and the sheet metal thickness ranges of deposition are 3~20nm, can also further pass through high temperature
(300~500 DEG C) annealing way controls the size of metal nanoparticle 6, and particle size range is selected from 10~300nm, metal material
Gold, silver, copper, aluminium.
Step S6: test substance 7 is placed on device by modes such as spraying, spin coatings.
Realization principle and desired effect of the invention are illustrated in conjunction with the embodiments further below.However, of the invention
It is not limited to the exemplary embodiment of following discloses, those skilled in the relevant arts can be subject to reality to it by different form
It is existing.The essence of specification is only to aid in those skilled in the relevant arts' Integrated Understanding detail of the invention.
The present embodiment is primarily based on magnetron sputtering and sinks in Si substrate by taking micron rectangle golden light grid and silver nano-grain as an example
Product 50nmAu and 300nmAl2O3, then it is prepared on same substrate using standard photolithography techniques and electron beam evaporation plating not collinear
Wide golden rectangular raster obtains a micron rectangle golden light grid-aluminium oxide-gold reflecting layer reflection-type micron antenna structure.The week of grating
Phase is fixed on 6 μm, and line width progressively increases to 3.6 μm from 2.0 μm with 0.4 μm of step-length, grating thickness 20nm.Fig. 5 (a) is provided
Period is P=6 μm, and the grating SEM that line width is w=3 μm schemes.Then it is grown on Cu foil by chemical vapor deposition (CVD)
Single-layer graphene, and use poly- (methyl methacrylate) (PMMA) as transfering reagent and transfer graphene to reflection-type micron
The surface of antenna optical grating construction.Finally, withEvaporation rate silver nano-grain is deposited on graphene, it is heavy by controlling
The partial size of product time control silver nano-grain.Fig. 5 (b) is the SEM figure of substrate after 5nm silver has been deposited.It can be seen from the figure that
There is no continuous film formings for silver, but at the nano particle of island.
Fig. 6 (a) is the grain size distribution of wherein substrate surface silver nano-grain.Pass through about 300 silver in statistics SEM figure
The diameter of nano particle, we calculate the average diameter of the substrate surface silver nano-grain is about 45nm.Utilize identical side
Method has obtained the silver nano-grain that partial size is 35nm and 55nm.Purple of the silver nano-grain being prepared in quartz plate substrate
Shown in outer visible absorption spectra such as Fig. 6 (b).It can be seen from the figure that silver nano-grain generates local under visible light wave excitation
Surface phasmon, to generate strong absorption in visible light wave range.With the increase of silver nano-grain partial size, resonance wave
Long that red shift occurs, when the average diameter of silver nano-grain is 45nm, the plasma peak of silver nano-grain is surveyed closest to Raman
Optical maser wavelength 532nm is tried, to can improve to maximum limitation the Raman active of device in spectrum test.
Fig. 7 (a) gives the Raman spectrums of double enhancing devices after vapor deposition silver nanoparticles with different particle diameters, can be with from figure
It is clearly observed the raman characteristic peak of graphene: 1580cm-1The peak G at place, 2685cm-1The peak 2D and 1334cm at place-1The D at place
Peak.The ratio at the peak 2D and the peak G is about 2 or so, and the peak D is unobvious, illustrates that the graphene in device is single-layer graphene, and
Without introducing biggish defect because of silver nano-grain is deposited on its surface.Meanwhile it can be seen from the figure that working as silver nanoparticle
When the average diameter of grain is about 45nm, silver nano-grain is maximum to the humidification of graphite Raman characteristic peak.
Embodiment is used as probe molecule using typical organic analysis object rhodamine 6G (R6G), its aqueous solution is sprayed to
On sample, then drying 2 minutes in air makes molecule be fixed on device surface.Fig. 7 (b) shows different molecular concentration
Average Raman spectrum of the R6G solution spraying on double enhancing devices, the average diameter of silver nano-grain is 45nm.It can be with from figure
Observe each raman characteristic peak of R6G, comprising: 1650,1574,1509,1362,1312,1182,772 and 612cm-1, with
Result reported in the literature is consistent.Meanwhile when molecular concentration is down to 10-12When M, the Raman signal of R6G still can be observed, count
Calculation obtains SERS enhancement factor up to 107, illustrate that double enhancing devices of preparation have good Raman reinforcing effect.
Fig. 8 (a) shows the reflectance spectrum of double enhancing devices under the conditions of different grating line widths.It can be seen from the figure that golden
Rectangular raster generates antenna resonance effect under infrared waves excitation, to generate strong absorption in infrared region；With line
Wide w progressively increases to 3.6 μm from 2.0 μm, and plasma peak is from 1350cm-1(7.4 μm) red shift is to 1050cm-1(9.5μm).Fig. 8
(b) reflectance spectrum of double enhancing devices when showing polyethylene oxide (PEO) as probe molecule is corresponded to.It can from figure
Out, a small amount of red shift has occurred relative to the curve of spectrum of naked device in the curve of spectrum of device after surface spin coating PEO.Meanwhile humorous
It shakes on peak it can be seen that apparent some protrusions, these protrusions indicate the various molecular vibrational modes of PEO molecule.Further pass through
Baseline Survey obtains the enhancing vibration signal curve of PEO molecule itself, as shown in Fig. 8 (c).It can be seen from the figure that preparation
Double enhancing devices are in 800~1500cm-1The each vibration mode of PEO molecule can be enhanced in frequency range, and work as PEO
When molecular vibrational frequency is close with the resonant frequency of metal micro antenna, double enhancing devices imitate PEO molecular vibration signal enhancing
Fruit is maximum.For example, for 1278cm-1The vibration mode at place, when grating line width be 2.4um when, plasma resonance frequency with should
Vibration mode is consistent, and double enhancing devices are maximum to the reinforcing effect of the mode.With the increase of grating line width, formant occurs red
It moves, causes plasma resonance frequency far from the vibration mode, reinforcing effect gradually decreases.Thus, by controlling optical grating construction
Parameter can carry out Selective long-range DEPT to PEO molecular vibrational mode, to realize that broadband detects.Double enhancing devices are calculated
8 × 10 are reached as high as to the enhancement factor of PEO infrared spectroscopy signals5。
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention rather than limits, although by upper
It states embodiment the present invention is described in detail, it should be appreciated to those skilled in the art that explanation and embodiment
Be regarded only as being exemplary, can make miscellaneous variation in the form and details, true scope of the invention and
Purport is defined in the claims.
Claims (10)
1. a kind of metallic graphite carbon alkene multilayer resonance structure enhances the infrared double spectra devices of Raman, it is characterised in that: including from lower
On the substrate, metallic reflector, dielectric layer, metal micro antenna, graphene film and the metal nanoparticle that set gradually；
It is anti-to form metal-dielectric-metal between the metal micro antenna and the metallic reflector for the dielectric layer
Emitting micron antenna structure, in the surface-reinforced infrared spectrum performance of infrared band enhancing device；
The graphene film forms nano gap between the metal nanoparticle and the metal micro antenna,
The Surface enhanced Raman spectroscopy performance of visible waveband enhancing device；
The metal micro antenna is the micron aerial array for the different structure that different zones design on dielectric layer, so that golden
The resonance peak for belonging to micron antenna is distributed in broadband infra-red range, and metal micro antenna generates antenna under infrared waves excitation
Resonance effect, so that strong local electric field is generated at metal micro antenna edge, when antenna resonant frequency and substance to be detected
When molecular vibrational frequency is consistent, greatly enhance the vibration signal intensity of tested molecule；Micron aerial array in each region
Figure is the same, specific size and the linear incremental variations of cycle parameter, shakes to realize in different zones to testing molecule difference
The Selective long-range DEPT and broadband of dynamic model formula detect；
The metal nanoparticle generates local surface phasmon under visible light wave excitation, thus in metal nano
Strong local electric field is generated around grain, further using graphene nano gap metal nanoparticle and metal micro antenna are sent out
Raw coupling, further increases the Surface enhanced Raman spectroscopy performance of device.
2. the infrared double spectra devices of enhancing Raman according to claim 1, it is characterised in that: the metal micro antenna
It is in rectangle, square, circle, ellipse, hexagon or crux in the transverse direction of device；The metal micro day
The size and periodic regime of line are 1 μm ~ 10 μm, and thickness range is 20 ~ 200nm.
3. the infrared double spectra devices of enhancing Raman according to claim 1, it is characterised in that: designed on the dielectric layer
The micron aerial array of different zones, each region correspond to a kind of micron antenna of size, so that micron antenna has one
Corresponding resonance peak, resonance wavelength λ realize antenna by designing the micron aerial array region of multiple parameters incremental variations
Resonance peak distribution in 3 ~ 16 μm of infra-red ranges；The areal is 2 ~ 10, and the areal extent in each region exists
Between 200 μm * 200 μm ~ 1mm*1mm.
4. the infrared double spectra devices of enhancing Raman according to claim 1, it is characterised in that: the graphene film is
1 ~ 10 layer.
5. the infrared double spectra devices of enhancing Raman according to claim 1, it is characterised in that: the metal nanoparticle
Particle size range be 10 ~ 300nm, metal material be selected from gold, silver, copper, aluminium.
6. the infrared double spectra devices of enhancing Raman according to claim 1, it is characterised in that: the thickness of the dielectric layer
Range are as follows: 20 ~ 1000nm forms reflection-type micron antenna structure between metal micro antenna and metallic reflector；It is described
The material of dielectric layer is infrared-transparent material, is selected from: Al2O3, KBr, MgF2, CaF2, BaF2, AgCl, ZnSe, SiO2, diamond-like
Stone carbon film.
7. enhancing the preparation method of the infrared double spectra devices of Raman described in claim 1, which is characterized in that comprising steps of
It prepares metallic reflector: one layer of metal layer is deposited on substrate, as reflecting layer；
Preparation media layer: the metallization medium layer on metallic reflector；
It prepares metal micro antenna: metal micro antenna being prepared using photoetching technique on dielectric layer；
Transfer graphene film: the graphene being prepared is transferred on metal micro antenna；
Prepare metal nanoparticle: the depositing metallic nanoparticles on graphene film.
8. enhancing the preparation method of the infrared double spectra devices of Raman according to claim 7, it is characterised in that: the gold
Belonging to micron antenna is using ultraviolet photolithographic, laser direct-write photoetching technology, in conjunction with electron beam evaporation plating, magnetron sputtering, hot evaporation method
It obtains.
9. enhancing the preparation method of the infrared double spectra devices of Raman according to claim 7, it is characterised in that: the stone
Black alkene film is prepared using mechanical stripping technique or chemical vapour deposition technique；The number of plies of the graphene film can be with
It is realized by directly growing multi-layer graphene or multiple branch mode.
10. enhancing the preparation method of the infrared double spectra devices of Raman according to claim 7, it is characterised in that: described
Metal nanoparticle is directly obtained by electron beam evaporation plating, magnetron sputtering, hot evaporation with slow 0.1 ~ 1/s of rate deposition；
The metal nanoparticle further passes through the size of 300 ~ 500 DEG C of annealing way control metal nanoparticles.
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| CN109612975B (en) * | 2018-12-07 | 2021-11-02 | 国家纳米科学中心 | Surface-enhanced Raman substrate and preparation method thereof |
| CN109765650A (en) * | 2019-02-28 | 2019-05-17 | 上海师范大学 | A method of the optical grating construction based on CD prepares SERS active-substrate |
| CN110098267A (en) * | 2019-04-09 | 2019-08-06 | 深圳激子科技有限公司 | A kind of graphene mid-infrared light detector and preparation method thereof based on the enhancing of phonon excimer |
| CN110534608A (en) * | 2019-08-02 | 2019-12-03 | 苏州众为光电有限公司 | A kind of reinforced graphite alkene near-infrared broadband light absorption structure and preparation method thereof |
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| CN114018304B (en) * | 2021-11-03 | 2024-05-07 | 北京理工大学 | Far infrared light layered sensor and preparation method thereof |
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