CN108226079A - The infrared double spectra devices of metallic graphite carbon alkene multilayer resonance structure enhancing Raman and preparation method - Google Patents
The infrared double spectra devices of metallic graphite carbon alkene multilayer resonance structure enhancing Raman and preparation method Download PDFInfo
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- G—PHYSICS
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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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- 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 enhances the infrared double spectra devices of Raman, including substrate, metallic reflector, dielectric layer, metal micro antenna, graphene film, metal nanoparticle.Dielectric layer forms metal medium metallic 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 in the range 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 the local electric field mode of resonance of high intensity, enhances the Raman scattering signal of trace molecules.The present invention has enhancing wide waveband, and enhancement factor is high, can large area processing, of low 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 to realize surface Raman light on individual devices
Spectrum and the device of the double enhancings of surface infrared absorption spectrum and preparation method thereof.
Background technology
Surface Enhanced spectral technique is that a kind of molecular spectrum to be grown up based on surface phasmon effect detects skill
Art is to determine the powerful tools of the important informations such as biomolecule composition and structure, in food security, 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 technologies can be with chemical in molecular detection
Polarizability change information caused by key chattering, and SEIRA technologies 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 pattern, the polarizability of molecule and dipole moment change information can not be obtained simultaneously.In order to which chemistry can be obtained comprehensively
The structural information of the numerous biomolecule of key chattering pattern, researcher combine the advantage of both technologies, it is proposed that
Surface Raman and the double enhancing technologies of infrared spectrum, realize the detection to molecular polarizability and dipole moment on the same base.At present
There are two types of resolving ideas.
First, preparing metal nanoparticle, local EMR electromagnetic resonance pattern 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. is prepared for nano grain of silver sub-island film, and realizes the SEIRA and SERS to ferroheme
Spectral detection.Monica Baia etc. have obtained self-assembling of gold nanoparticles using successive sedimentation method, realize p-aminophenyl thiophenol
SERS the and SEIRA spectral signals detection of molecule.Jiannian Yao etc. assemble netted gold nano grain, to being tested molecule
SERS enhancement factors are 106, SEIRA enhancement factors are 102.Although such method be successfully realized on the same chip SERS with
The double enhancings of SEIRA spectrum, but the enhancing effect of infrared band SEIRA is poor, enhancement factor is only 102。
Second is that design metal nano antenna, local EMR electromagnetic resonance pattern is generated in visible and infrared two wave bands.2013,
Cristiano D ' Andrea etc. devise gold nano antenna structure array using electron beam lithography, by changing exciting field
Polarization direction infrared band excitation antenna antenna resonance effect, so as to generate the sharp local EMR electromagnetic resonance of high intensity
Peak.This method has increased substantially 6 × 10 to the SEIRA enhancement factors of methylene cyan molecule5.However, it is completed in device fabrication
Afterwards, resonant frequency immobilizes.Infrared signature fingerprint region during narrow spectrum enhancing wave band can not cover so that the device is only
SEIRA spectral detections can be carried out to a few molecules.Meanwhile the SERS enhancement factors of the substrate only have 102。
In conclusion although both the above method can realize the Raman signal and infrared absorption spectrum to test substance
Double enhancing effects of signal, still, they are all that enhancement factor is cost to sacrifice one of them (SERS or SEIRA), nothing
Method ensures that Raman signal and infrared spectroscopy signals all have high enhancement factor.
Invention content
The present invention proposes a kind of based on the enhancing drawing of metallic graphite carbon alkene multilayer resonance structure for overcome the deficiencies in the prior art
Metal nanoparticle with metal micro antenna is combined, excites metal nano respectively by graceful infrared double spectra devices and preparation method
Particle visible light wave range local plasmon bulk effect and metal micro antenna infrared band antenna resonance effect, so as to
It realizes double enhancing 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, available for fields such as environmental monitoring, food securities.
The technical issues of to solve the present invention, used technical solution is：
The infrared double spectra devices of Raman are enhanced based on metallic graphite carbon alkene multilayer resonance structure, including setting 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 performances of infrared band enhancing device.
The graphene film is formed between the metal nanoparticle and the metal micro antenna between nanometer
Gap, in the SERS performances 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 there are one specific resonance peak (corresponding resonance wavelengths for micron antenna tool
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) realize that the resonance peak of antenna is distributed in 3~16 μm of infra-red ranges, it can
To generate antenna resonance effect under being excited in infrared waves, so as 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 so as to be realized 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, to generate local surface phasmon under visible light wave excitation, so as in metal
Strong local electric field is generated around nano particle, further causes metal nanoparticle and metal micro using graphene nano gap
Antenna couples, and improves the SERS performances 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 it is rectangular, square, round, oval in the transverse direction of device,
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, positioned 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 may be selected from：Al2O3, KBr, MgF2,
CaF2, BaF2, AgCl, ZnSe, SiO2, diamond-like carbon film.
Present invention further propose that enhance the preparation method of the infrared double spectra devices of Raman above.Include the following steps：
(1) metallic reflector is prepared：One layer of metal layer is deposited on sinking to the bottom 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, with reference to electron beam evaporation plating, magnetic
The methods of control sputters, hot evaporation deposited metal micron antenna on dielectric layer.
(4) graphene film is shifted：Using 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；Also can further 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 selects
From gold, silver, copper, aluminium.
Relative to the prior art, the invention has the advantages 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 of metaplasia production.
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 is imitated using the reflection-type micron antenna structure method amber resonance that reflecting surface is formed up and down
Should, the local to infrared waves is further enhanced, so as to fulfill the maximum enhancing 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, make its generation humorous
It shakes pattern, is detected so as to fulfill enhancing the broadband of test substance.
Third, for graphene as a kind of two-dimensional material, thickness only has 0.34nm, and the present invention is by the use of 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
On direction there is the Mode Coupling between nano particle, while there is metal nanoparticle and metal micro day in vertical direction
Coupling between line, so as to greatly enhance the SERS performances 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 also needing to remake device and sample when avoiding replacement measuring method, it can realize 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.
Description of the drawings
Fig. 1 enhances the infrared double spectra device schematic diagrames of Raman for metallic graphite carbon alkene multilayer resonance structure；
Fig. 2 is the schematic diagram for including multiple and different regions on same device；
Fig. 3 (a)-Fig. 3 (f) is rectangle, and square, disc is oval, hexagon, the metal micro day of crux
Line schematic diagram；
The schematic three dimensional views of Fig. 3 (g) is section when being square metal micro antenna；
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 the SEM pictures of micron rectangle golden light grid/aluminium oxide/gold reflecting layer reflection-type micron antenna structure；
Fig. 5 (b) is the SEM pictures 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 molecules after Baseline Survey.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with the accompanying drawings to the present invention's
Preferred embodiment is described in further detail.Identical reference numeral 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.During test, detection substance 7 to be measured is placed in by modes such as spraying, spin coatings on device.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
Enclose for：20~1000nm, the material of dielectric layer is infrared-transparent material, be may 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, positioned at the metal nanoparticle 6
Between the metal micro antenna 4, nano gap is formed, metal nanoparticle is made to be coupled with metal micro antenna, is carried
The SERS performances 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 more than structure, metal micro antenna 4 can generate antenna resonance effect under infrared waves excitation, so as in gold
Belong to 4 edge of micron antenna and generate 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 so as to be realized in different zones.Metal nano
Local surface phasmon can be generated under visible light wave excitation by visiting particle 6, strong so as to be generated around metal nanoparticle 6
Local electric field further causes metal nanoparticle 6 to be coupled with metal micro antenna 4, carries using graphene nano gap
The SERS performances of high device.By the infrared vibration signal and Raman scattering signal that separately detect test substance 7, you can to be measured
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
Corresponding a kind of micron antenna of specific dimensions so that there are one specific resonance peak for micron antenna tool (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.Resonance peak to realize 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 schematic three dimensional views of the section for the micron antenna structure of square.Gold
It is 1 μm~10 μm to belong to the size of micron antenna and periodic regime, 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：Prepare metallic reflector.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：Prepare metal micro antenna.Using microlithography technologies such as ultraviolet photolithographic, laser direct-writings, with reference to electron beam
The methods of vapor deposition, magnetron sputtering, hot evaporation the deposited metal micron antenna 4 on dielectric layer.The shape of metal micro antenna 4 can be with
Select the one or more of which 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：Shift 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：Prepare metal nanoparticle.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, also can 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.
The realization principle and desired effect of the present invention are illustrated in conjunction with the embodiments further below.It is however, of the invention
The exemplary embodiment of following discloses is not limited to, various equivalent modifications can be subject to reality by different form to it
It is existing.The essence of specification is only to aid in the detail of the various equivalent modifications Integrated Understanding present invention.
The present embodiment is primarily based on magnetron sputtering and sinks in Si substrates 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 foils 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 grain size of product time control silver nano-grain.Fig. 5 (b) is the SEM figures that substrate after 5nm silver has been deposited.It can be seen from the figure that
Silver is there is no continuous film forming, but into the nano particle of island.
Fig. 6 (a) is the grain size distribution of wherein substrate surface silver nano-grain.By counting about 300 silver in SEM figures
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 grain 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, so as to generate strong absorption in visible light wave range.With the increase of silver nano-grain grain 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, so as 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 G peaks at place, 2685cm-1The 2D peaks and 1334cm at place-1The D at place
Peak.2D peaks and the ratio at G peaks are about 2 or so, and D peaks unobvious, and it is single-layer graphene to illustrate the graphene in device, and
Without introducing the defects of larger because of silver nano-grain is deposited on its surface.Meanwhile it can be seen from the figure that when silver nanoparticle
When the average diameter of grain is about 45nm, silver nano-grain is maximum to the humidification of graphite Raman characteristic peak.
As probe molecule, its aqueous solution is sprayed to using typical organic analysis object rhodamine 6G (R6G) for embodiment
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 sprayings 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, including：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 10-12During M, the Raman signal of R6G still can be observed, count
Calculation obtains SERS enhancement factors up to 107, illustrate that the double enhancing devices prepared have good Raman enhancing effect.
Fig. 8 (a) shows the reflectance spectrum of double enhancing devices under the conditions of different grating line widths.It is it can be seen from the figure that golden
Rectangular raster generates antenna resonance effect under infrared waves excitation, so as 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 spectrums of double enhancing devices when showing polyethylene oxide (PEO) as probe molecule are corresponded to.It can from figure
Go 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 some apparent protrusions, these protrusions represent the various molecular vibrational modes of PEO molecules.Further pass through
Baseline Survey obtains the enhancing vibration signal curve of PEO molecules in itself, as shown in Fig. 8 (c).It can be seen from the figure that prepare
Double enhancing devices are in 800~1500cm-1The each vibration mode of PEO molecules can be enhanced, and work as PEO in frequency range
When molecular vibrational frequency is close with the resonant frequency of metal micro antenna, double enhancing devices imitate PEO molecular vibrations signal enhancing
Fruit is maximum.For example, for 1278cm-1The vibration mode at place, when grating line width is 2.4um, plasma resonance frequency is with being somebody's turn to do
Vibration mode is consistent, and double enhancing devices are maximum to the enhancing effect of the pattern.With the increase of grating line width, formant occurs red
It moves, leading to plasma resonance frequency, enhancing effect continuously decreases far from the vibration mode.Thus, by controlling optical grating construction
Parameter can carry out Selective long-range DEPT to PEO molecular vibrational modes, be detected so as to fulfill broadband.Double enhancing devices are calculated
8 × 10 are reached as high as to the enhancement factor of PEO infrared spectroscopy signals5。
Finally illustrate, above example is merely to illustrate technical scheme of the present invention and unrestricted, 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 and
On the substrate, metallic reflector, dielectric layer, metal micro antenna, graphene film and the metal nanoparticle that set gradually；
Between the metal micro antenna and the metallic reflector, it is anti-to form metal-dielectric-metal for the dielectric layer
Emitting micron antenna structure, in the surface-reinforced infrared spectrum performance of infrared band enhancing device；
The graphene film between the metal nanoparticle and the metal micro antenna, forms nano gap,
Visible waveband enhances the Surface enhanced Raman spectroscopy performance of device；
The metal micro antenna is the micron aerial array of the different structure that different zones design on dielectric layer so that gold
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 as to generate strong local electric field at metal micro antenna edge, when antenna resonant frequency and substance to be detected
When molecular vibrational frequency is consistent, greatly enhancing is tested the vibration signal intensity of molecule；Micron aerial array in each region
Figure is the same, specific size and the linear incremental variations of cycle parameter, so as to shake in different zones realization to testing molecule difference
Selective long-range DEPT and the broadband detection of dynamic model formula；
The metal nano visits particle, local surface phasmon is generated under visible light wave excitation, so as in metal nano
Strong local electric field is generated around particle, further causes metal nanoparticle and metal micro antenna using graphene nano gap
It couples, further improves the Surface enhanced Raman spectroscopy performance of device.
2. the enhancing infrared double spectra devices of Raman according to claim 1, it is characterised in that：The metal micro antenna exists
Rectangular, square, round, oval, hexagon or crux in the transverse direction of device；The metal micro antenna
Size and periodic regime be 1 μm~10 μm, thickness range be 20~200nm.
3. the enhancing infrared double spectra devices of Raman according to claim 1, it is characterised in that：It is designed not on the dielectric layer
With the micron aerial array in region, each region corresponds to a kind of micron antenna of size so that there are one right for micron antenna tool
The resonance peak answered, resonance wavelength λ realize antenna by designing the micron aerial array region of multiple parameters incremental variations
Resonance peak is distributed in 3~16 μm of infra-red ranges；The areal is 2~10, and the areal extent in each region is in 200 μ
Between m*200 μm~1mm*1mm.
4. the enhancing infrared double spectra devices of Raman according to claim 1, it is characterised in that：The graphene film is 1
~10 layers.
5. the enhancing infrared double spectra devices of Raman according to claim 1, it is characterised in that：The metal nanoparticle
Particle size range is 10~300nm, and metal material is selected from gold, silver, copper, aluminium.
6. the enhancing infrared double spectra devices of Raman according to claim 1, it is characterised in that：The thickness model of the dielectric layer
Enclose for：20~1000nm forms reflection-type micron antenna structure between metal micro antenna and metallic reflector；It is given an account of
The material of matter layer is infrared-transparent material, is selected from：Al2O3, KBr, MgF2, CaF2, BaF2, AgCl, ZnSe, SiO2, diamond-like
Carbon film.
7. the preparation method of the enhancing infrared double spectra devices of Raman described in claim 1, which is characterized in that including step：
(1) metallic reflector is prepared：One layer of metal layer is deposited on substrate, as reflecting layer；
(2) preparation media layer：The metallization medium layer on metallic reflector；
(3) metal micro antenna is prepared：Metal micro antenna is prepared using photoetching technique on dielectric layer；
(4) graphene film is shifted：The graphene being prepared is transferred on metal micro antenna；
(5) metal nanoparticle is prepared：The depositing metallic nanoparticles on graphene film.
8. the preparation method of the enhancing infrared double spectra devices of Raman according to claim 7, it is characterised in that：The metal
Micron antenna is using photoetching techniques such as ultraviolet photolithographic, laser direct-writings, with reference to the side such as electron beam evaporation plating, magnetron sputtering, hot evaporation
Method obtains.
9. the preparation method of the enhancing infrared double spectra devices of Raman according to claim 7, it is characterised in that：The graphite
Alkene film is prepared using mechanical stripping technique or chemical vapour deposition technique；The number of plies of the graphene film can lead to
It crosses directly growth multi-layer graphene or multiple branch mode is realized.
10. the preparation method of the enhancing infrared double spectra devices of Raman according to claim 7, it is characterised in that：The gold
Metal nano-particle is by electron beam evaporation plating, magnetron sputtering, hot evaporation with slow rateDeposition directly obtains；It is described
Metal nanoparticle further controls the size of metal nanoparticle by 300~500 ° of annealing way.
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