CN106596449B - Infrared graphene plasmon biochemical sensor in one kind - Google Patents
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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
- G01N21/17—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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- 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
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- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
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Abstract
The invention discloses graphene plasmon biochemical sensor infrared in one kind, infrared wide spectrum light source, Infrared Lens in first, Infrared Lens in graphene plasmon sensing unit and second including in；Graphene plasmon sensing unit includes doped silicon substrate, the first, second grating coupled zone, sensing unit and the graphene layer being covered on above the first, second grating coupled zone and sensing unit；The mid-infrared light wave that wide spectrum light source issues focuses on the first grating coupled zone by Infrared Lens in first and couples with graphene plasmon, infrared graphene plasmon passes through graphene layer to sensing unit in generating, through, to the second grating coupled zone, scattering to far field by graphene layer after being reacted repeatedly with biological sample thereon；Progress spectral measurement analysis in Fourier infrared spectrograph is focused on by Infrared Lens in second.Infrared graphene plasmon is reacted in sensing unit with biological sample repeatedly in the present invention, improves the sensitivity of biomolecule detection.
Description
Technical field
The present invention relates to optical sensing fields, and in particular to infrared graphene plasmon biochemical sensor in one kind.
Background technique
For middle infrared band (3-30 microns) by special applications on biochemical sensitive, this wave band covers the vibrational energy of molecule
Grade can be used to the biochemical basic structural unit of identification and analysis life, such as protein, fat, DNA.Mid infrared absorption spectrum
Technology can be absorbed by the fingerprint of molecular resonance, non-intrusion type, the unmarked Biochemical Information for obtaining substance.However due to life
The mismatch of size (usually less than 10 nanometers) and middle infrared wavelength of chemoattractant molecule, the absorption of vibrations for resulting in molecule are very micro-
Weak, this is very unfavorable for the detection of nanoscale molecule, absorbs weak limitation, locally resonant metal Nano structure to overcome
It is applied to molecular detection, enhances molecular detection sensitivity.Although metal nano resonance can enhance nanoscale molecular detection
Sensitivity, but due to metal in middle infrared band similar to electronics perfection conductor, the electron interaction in photon and metal is very
Weak, metal nano resonance technique is still limited by relatively weak optical enhancement and non-tunable narrow-band spectrum.
Graphene is according to the carbon atom of honeycomb two-dimensional arrangements, and because of its brilliant electrical and optical performance, it is known as photon
It learns and the revolutionary material of photoelectronics.Graphene plasmon (graphene plasmons) is photon-driven graphene
The collective of middle electronics shakes, and is a kind of electromagnetic wave, and compared with the plasmon of traditional metal structure, graphene plasma swashs
Member has three aspect characteristic advantages:
(1) carrier concentration of doped graphene can realize the big model of high speed by the bias of field-effect tube (FET) very little
The modulation enclosed, switch time were shorter than for 1 nanosecond, this is very crucial for the opto-electronic device for realizing high speed；
(2) wavelength of graphene plasmon 1-3 magnitude smaller than free space optical wavelength, this means that graphene
Plasmon has very strong restriction effect to mid-infrared light field, can greatly enhance the interaction of light and substance；
(3) graphene plasmon recovery time is longer, compared with metal plasma excimer, graphene plasmon
Distance relatively far away from can be transmitted.
In conclusion we can replace metal plasma excimer with graphene plasmon, middle infrared absorption is utilized
Spectral technique and graphene plasmon characteristic superiority enhance the absorption of vibrations to nanoscale biomolecule, to realize
The high-acruracy survey that super-small chip absorbs the refractive index and vibration fingerprint of different classes of biomolecule.
Summary of the invention
The technical problem to be solved by the present invention is to special using mid infrared absorption spectrum technology and graphene plasmon
Sign advantage enhances the absorption of vibrations to nanoscale biomolecule, to realize super-small chip to different classes of biology point
The problem of high-acruracy survey that the refractive index and vibration fingerprint of son absorb.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that provide in one kind infrared graphene etc. from
Sub- excimer biochemical sensor, infrared wide spectrum light source, Infrared Lens, graphene plasmon sensing unit in first including in
With second in Infrared Lens；
The graphene plasmon sensing unit includes doped silicon substrate, is laid in the doped silicon substrate two respectively
The first grating coupled zone and the second grating coupled zone at end, the sensing unit being laid among the doped silicon substrate, and covering
Graphene layer above first grating coupled zone, sensing unit and the second grating coupled zone；
The mid-infrared light wave that infrared wide spectrum light source issues in described focuses on described the by Infrared Lens in described first
One grating coupled zone, couples with graphene plasmon, infrared graphene plasmon in generation；Infrared graphite in described
Alkene plasmon reaches the sensing unit by the graphene layer, repeatedly with the biological sample that is placed on the sensing unit
Reaction；Second grating coupled zone is reached via the graphene layer again, and scatters to far field；By infrared in described second
Mirror focuses on progress spectral measurement analysis in infrared spectrometer.
In the above scheme, the screen periods length Λ of first grating coupled zone and the second grating coupled zone are as follows:
Λ=λ0/neff；
Wherein, λ0It is free space mid-infrared light wavelength；neffEffective refraction of infrared graphene plasmon in being
Rate.
In the above scheme, the sensing unit is optical microcavity structure, including is laid in the doped silicon lining laterally side by side
Two identical Bragg reflectors on bottom；
Each Bragg reflector includes M air ducting layer and doped silicon ducting layer, and by first air ducting layer
The sequence of doped silicon ducting layer is transversely alternately arranged afterwards, 8 >=M >=4；
By an air grooves connection among two Bragg reflectors, an optical resonator is formed, two
The Bragg reflector make in infrared graphene plasmon height local in the air grooves, it is described with being filled in
The biological sample of air grooves repeated reaction.
In the above scheme, the grating of first grating coupled zone and the second grating coupled zone is by the doping
Linear groove is etched on silicon substrate to realize；
The air ducting layer of the Bragg reflector and the air grooves are by the doped silicon substrate
Linear double Prague emitting structural grooves are etched to realize.
In the above scheme, the lateral length d1 of the air ducting layer of the Bragg reflector and doped silicon ducting layer
Lateral length d2 determines by Bragg condition, physical relationship are as follows:
d1×Real(neff1)+d2×Real(neff2)=m λb/2；
Wherein, λbIt is the central wavelength in Prague；M is the order in Prague；Real(neff1) be in infrared graphene etc. from
Effective refractive index of the sub- excimer in air ducting layer；Real(neff2) be in infrared graphene plasmon in doped silicon waveguide
The effective refractive index of layer.
In the above scheme, the lateral length L of the air grooves of two Bragg reflectors is connected are as follows:
L=Λ r/ [neff·2]；
Wherein, Λ r is resonant wavelength；neffIt is the effective refractive index of resonant wavelength waveguide.
In the above scheme, the graphene plasmon sensing unit further includes dielectric layer, the dielectric layer setting
Between the graphene layer and the doped silicon substrate, field-effect tube structure is formed；
The graphene layer is equipped with metal electrode, the metal electrode ground connection；
When the doped silicon substrate connects electricity, field-effect tube structure conducting applies voltage for the graphene layer；
The size for being applied to voltage on the graphene layer is adjusted, the fermi level size of graphene is adjusted, graphene
Fermi level size changes resonance spectrum and moves.
In the above scheme, the dielectric layer is Al2O3。
The present invention utilize in infrared graphene plasmon the characteristics of optical resonator reacts repeatedly with biological sample,
Enhance to the absorption of vibrations of nanoscale biomolecule, realize super-small chip to the refractive index of different classes of biomolecule and
High-acruracy survey while vibration fingerprint absorbs, improves the sensitivity of biomolecule detection and the integrated level of sensor.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of infrared graphene plasmon biochemical sensor in one kind provided by the invention；
Fig. 2 is the structural schematic diagram of graphene plasmon sensing unit in the present invention；
Fig. 3 is to use the spectrum test result signal that infrared plasmon biochemical sensor obtains in provided by the invention
Figure.
Specific embodiment
The present invention light field constraint and tunable characteristic superpower using graphene plasmon, in highly integrated core
On piece realizes complex refractivity index and spectrum the high-precision detection simultaneously to the micro biochemicals material such as protein.
The present invention is described in detail with specific embodiment with reference to the accompanying drawings of the specification.
As shown in Figure 1, it is provided by the invention one kind in infrared graphene plasmon biochemical sensor, including in it is infrared
Wide spectrum light source (globar) 10, first in Infrared Lens 20, infrared in graphene plasmon sensing unit 30 and second
Lens 40；Graphene plasmon sensing unit 30 includes doped silicon substrate 35, is laid in 35 both ends of doped silicon substrate respectively
The first grating coupled zone 31 and the second grating coupled zone 34, the sensing unit 33 that is laid among doped silicon substrate 35, and cover
The graphene layer 32 above the first grating coupled zone 31, sensing unit 33 and the second grating coupled zone 34 is covered, in the present invention, the
One, the second grating coupled zone is made of diffraction grating；
In the free space mid-infrared light wave that issues of infrared wide spectrum light source 10 by Infrared Lens 20 in first focus on stone
On first grating coupled zone 31 of black alkene plasmon sensing unit 30, coupled with graphene plasmon, it is red in generation
Outer graphene plasmon；In infrared graphene plasmon by waveguide media graphene layer 32 reach sensing unit 33,
After reacting repeatedly with the biological sample (such as protein) being placed on sensing unit 33, the second grating is reached via graphene layer 32
Coupled zone 34, and scatter to far field；Fourier Transform Infrared Spectrometer 50 (FTIR) is focused on by Infrared Lens 40 in second again
Middle progress spectral measurement analysis.
Big 1-2 amount of the transmission wave vector of infrared graphene plasmon than free space mid-infrared light wave due in
Grade, there are great wave vector mismatch between them, cannot directly by free space mid-infrared light wave be coupled to graphene etc. from
Sub- excimer converts infrared graphene plasmon in generating, and therefore, the present invention uses grating (the first, second light of sub-wavelength
The grating of grid coupled zone) compensate the mismatch of wave vector.The screen periods length Λ of first, second grating coupled zone of the invention
Are as follows:
Λ=λ0/neff；
Wherein, λ0It is free space mid-infrared light wavelength, in the present invention, we are using wideband light source, λ0It takes wherein
Cardiac wave is long, still can keep very big coupling efficiency；neffThe effective refractive index of infrared graphene plasmon in being.
As shown in Fig. 2, in the present invention, sensing unit 33 is optical microcavity structure, including laterally (by the first grating coupled zone
The direction of 31 to the second grating coupled zone 34) it is laid in two identical Bragg reflectors in doped silicon substrate 35 side by side
331, each Bragg reflector 331 includes M air ducting layer 3311 and doped silicon ducting layer 3312, and by first air waveguide
The sequence of layer 3311 and rear doped silicon ducting layer 3312 is transversely alternately arranged, and M >=4, M is bigger, and measurement accuracy is higher, while by
In the limitation of the first transmission range of graphene plasma excitement, M value is no more than 8；Pass through among two Bragg reflectors 331
One air grooves 332 connects, and forms an optical resonator；The grating of first, second grating coupled zone of the invention is logical
It crosses and etches linear groove realization in doped silicon substrate 35, the air ducting layer 3311 and air of Bragg reflector 331 are recessed
Slot 332 is realized by etching double Prague emitting structural grooves in doped silicon substrate 35.
Two Bragg reflectors 331 make in infrared graphene plasmon height local in 332 (optics of air grooves
Resonant cavity) in, it repeated and react with the biological sample for being filled in air grooves 332, so that high-precision measure biological sample
The drift of the infrared spectroscopy and formant of molecule.
In the present invention, the air ducting layer of Bragg reflector 331 lateral length d1 (in infrared graphene plasma
Excimer is in the conveying length in air waveguide) with the lateral length d2 of doped silicon ducting layer (in infrared graphene plasmon
In the conveying length of doped silicon ducting layer) it is determined by Bragg condition, it may be assumed that
d1×Real(neff1)+d2×Real(neff2)=m λb/2；
Wherein, λbIt is the central wavelength in Prague；M is the order in Prague；Real(neff1) be in infrared graphene etc. from
Effective refractive index of the sub- excimer in air ducting layer；Real(neff2) be in infrared graphene plasmon in doped silicon waveguide
The effective refractive index of layer.
Connect the long L (air grooves of chamber of the optical resonator of the formation of air grooves 332 of two Bragg reflectors 331
Lateral length) are as follows:
L=Λ r/ [neff·2]；
Wherein, Λ r is resonant wavelength；neffIt is the effective refractive index of resonant wavelength waveguide, it is graphene fermi level Ef
Function, graphene fermi level can be regulated and controled by adjusting the voltage that is applied on graphene.
In the present invention, graphene plasmon sensing unit 30 further includes dielectric layer 36, and dielectric layer 36 is arranged in stone
Between black alkene layer 32 and doped silicon substrate 35, field-effect tube structure is formed；Present media layer 36 is Al2O3, in Al2O3In, in
Infrared graphene plasmon transmission loss is small.
In the present invention, metal electrode 37 is equipped on graphene layer 32, metal electrode 37 is grounded, and doped silicon substrate 35 connects
Electricity, field-effect tube structure conducting realize that the mode of back electrode power-up is that graphene layer 32 applies voltage, are applied to stone by adjusting
Voltage swing on black alkene layer 32, regulation are the fermi level sizes of graphene, and resonance spectrum is big with the fermi level of graphene
Small change is moved；When resonance spectrum occurs mobile, formant will be in different wavelength regions, to realize to not jljl
The measurement of the absorption peak of matter thus can measure different biological samples on a biochemical sensor.
Fig. 3 is to use the spectrum test result signal that infrared plasmon biochemical sensor obtains in provided by the invention
Figure, in infrared plasmon biochemical sensor predominantly detect the movement of formant and two physical quantitys of absorption of formant.By
The characteristic of infrared Plasmon Resonance enhancing, (in Fig. 3, is applied on graphene by the wavelength amount of movement of formant in
Voltage when being V1, the wavelength amount of movement of formant is Δ λ 1；When the voltage being applied on graphene is V2, the wavelength of formant
Amount of movement is Δ λ 2), highly sensitive the refractive index of biomolecule can be obtained, can be given birth to high precision by formant absorption
The fingerprint of object molecule absorbs information, and (when the voltage being applied on graphene in Fig. 3 is V1, formant is absorbed as absorption peak 1；Apply
When the voltage on graphene is V2, formant is absorbed as absorption peak 2；), to judge that protein types and denaturation etc. are important
Biometric information.Using the characteristic of the fermi level electric tunable of graphene, by the voltage being applied on graphene from V1 tune
V2 is saved, the formant dynamic of graphene can be continuously regulated to different positions, to measure the refraction of different biological molecules
Rate and fingerprint absorption spectrum.
In the present invention, the manufacture craft of graphene plasmon sensing unit includes the following steps:
Commonly lightly doped silicon wafer (1-10 Ω cm) is used as graphite using semiconductor technology for the first step, device of the present invention
The substrate of alkene plasmon sensing unit is drawn and takes the doped silicon wafer of 1cm*1cm as doped silicon substrate 10.
PMMA (poly methyl methacrylate) photoresist is uniformly spin-coated in doped silicon substrate 10 by second step
Face after drying, is put into electron beam exposure instrument, design configuration is transferred in doped silicon substrate 10.
Third step will not be photo-etched glue guarantor using reactive ion light beam etching machine (reactive ion etching RIE)
The silicon dry etching in shield region falls 20nm.Then the doped silicon substrate 10 after etching is put into acetone soln, thoroughly removes and covers
Cover the PMMA photoresist on surface.
4th step, using thermal evaporation instrument under conditions of high vacuum low rate, slowly be deposited one layer of 30nm three oxidations
Two aluminium (Al2O3) as the dielectric layer applied backwards to voltage (back electrode).
5th step, using commercial chemical vapour deposition technique (chemical vapor deposition CVD) in copper film
Graphene is laid on substrate.Before shifting grapheme two-dimension material, first by spin coating one uniform above the graphene layer of copper film
PMMA layers of layer, then puts it into iron chloride (ferric chloride) environment and impregnates 12 hours, make the substrate of copper completely molten
It takes off；The graphene film for being suspended in corrosive liquid surface and being stamped PMMA is got and is put into distilled water repeatedly rinsing until corrosion
Until residue is cleaned out；Then the graphene sample insertion after etching pattern is floated on and is covered with PMMA layers of graphene film
In the following, carefully scoop up, allow the uniform unfolded of graphene film is layered on graphene sample area of the pattern in doped silicon substrate 10；Deng
After graphene sample is dry, it is put into acetone soln and isopropanol and removes PMMA layers.
After the graphene sample shifted is again passed by electron beam exposure, the titanium and 100nm gold of 5nm is deposited, then exists
Removing is carried out in acetone soln and forms electrode 13, and so far, entire graphene plasmon sensing unit preparation finishes.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (7)
1. infrared graphene plasmon biochemical sensor in one kind, which is characterized in that infrared wide spectrum light source, including in
Infrared Lens in one, Infrared Lens in graphene plasmon sensing unit and second；
The graphene plasmon sensing unit includes doped silicon substrate, is laid in the doped silicon substrate both ends respectively
First grating coupled zone and the second grating coupled zone, the sensing unit being laid among the doped silicon substrate, and it is covered on institute
State the graphene layer above the first grating coupled zone, sensing unit and the second grating coupled zone；
The mid-infrared light wave that infrared wide spectrum light source issues in described focuses on first light by Infrared Lens in described first
Grid coupled zone is coupled with graphene plasmon, infrared graphene plasmon in generation；Infrared graphene etc. in described
Ion excimer reaches the sensing unit by the graphene layer, repeatedly anti-with the biological sample that is placed on the sensing unit
It answers；Second grating coupled zone is reached via the graphene layer again, and scatters to far field；By Infrared Lens in described second
Focus on progress spectral measurement analysis in infrared spectrometer；
The sensing unit is optical microcavity structure, including two identical cloth being laid in the doped silicon substrate laterally side by side
Bragg reflector；
Each Bragg reflector includes M air ducting layer and doped silicon ducting layer, and by mixing after first air ducting layer
The sequence of miscellaneous silicon ducting layer is transversely alternately arranged, 8 >=M >=4；
By an air grooves connection among two Bragg reflectors, an optical resonator is formed, described in two
Bragg reflector make in infrared graphene plasmon height local in the air grooves, and be filled in the air
The biological sample of groove repeated reaction.
2. sensor as described in claim 1, which is characterized in that first grating coupled zone and the second grating coupled zone
Screen periods length Λ are as follows:
Λ=λ0/neff；
Wherein, λ0It is free space mid-infrared light wavelength；neffThe effective refractive index of infrared graphene plasmon in being.
3. sensor as described in claim 1, which is characterized in that first grating coupled zone and the second grating coupled zone
Grating is realized by etching linear groove in the doped silicon substrate；
The air ducting layer of the Bragg reflector and the air grooves are by etching in the doped silicon substrate
Linear double Prague emitting structural grooves are realized.
4. sensor as described in claim 1, which is characterized in that the transverse direction of the air ducting layer of the Bragg reflector is long
Degree d1 and doped silicon ducting layer lateral length d2 determined by Bragg condition, physical relationship are as follows:
d1×Real(neff1)+d2×Real(neff2)=m λb/2；
Wherein, λbIt is the central wavelength in Prague；M is the order in Prague；Real(neff1) be in infrared graphene plasma swash
Effective refractive index of the member in air ducting layer；Real(neff2) be in infrared graphene plasmon in doped silicon ducting layer
Effective refractive index.
5. sensor as described in claim 1, which is characterized in that the air grooves of two Bragg reflectors of connection
Lateral length L are as follows:
L=Λ r/ [neff·2]；
Wherein, Λ r is resonant wavelength；neffIt is the effective refractive index of resonant wavelength waveguide.
6. sensor as described in claim 1, which is characterized in that the graphene plasmon sensing unit further includes being situated between
Matter layer, the dielectric layer are arranged between the graphene layer and the doped silicon substrate, form field-effect tube structure；
The graphene layer is equipped with metal electrode, the metal electrode ground connection；
When the doped silicon substrate connects electricity, field-effect tube structure conducting applies voltage for the graphene layer；
The size for being applied to voltage on the graphene layer is adjusted, the fermi level size of graphene, the Fermi of graphene are adjusted
Energy level size changes resonance spectrum and moves.
7. sensor as claimed in claim 6, which is characterized in that the dielectric layer is Al2O3。
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| US11688820B2 (en) | 2019-10-10 | 2023-06-27 | Regents Of The University Of Minnesota | Photodetectors |
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