CN206756692U - Without frequency conversion cubical array plasma resonance sensor - Google Patents
Without frequency conversion cubical array plasma resonance sensor Download PDFInfo
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- CN206756692U CN206756692U CN201720553346.3U CN201720553346U CN206756692U CN 206756692 U CN206756692 U CN 206756692U CN 201720553346 U CN201720553346 U CN 201720553346U CN 206756692 U CN206756692 U CN 206756692U
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Abstract
The utility model provides one kind without frequency conversion cubical array plasma resonance sensor, including plasma resonance substrate, for the array of cavities of nanostructured, multi-layered material structure layer is covered thereon, including the first metal layer, insulating barrier and second metal layer arranged successively from bottom to up, the multi-layered material structure layer forms the optical resonator array being embedded in the plasma resonance sensor in substrate, and the optical resonator is the cavity of tapered cups.It is limited to solve prior art plasma resonance sensor detection sensitivity, and the large-scale not readily portable technical problem of device, hypersensitive, label-free biomolecule detection are realized, to realize that opening for the portable medical biology sensor of early detection disease biomarker provides basis.
Description
Technical field
The utility model is related to sensor and field of sensing technologies, especially, be related to it is a kind of without frequency conversion cubical array etc. from
Sub-resonance sensor.
Background technology
Surface plasmon resonance (Surface Plasmon Resonance, SPR) is the freely electricity by metal surface
Son and the interaction of electromagnetic wave (light) and caused covibration, by the use of the technology as detecting the biomolecule such as protein
The method of interaction.Applications of surface plasmon resonance (SPR) is used for by nineteen eighty-three, Sweden scientist Liedberg first
The measure of IgG antibody and its antigen interactions.Then the technology penetrates into basic life science research quickly.SPR technique
Molecule need not be marked with it and consume the advantages of sample is minimum as a kind of ripe measurement biological disperser
Method.In addition, another focus of drug screening and its identification and SPR technique application.Compared with fluoroscopic examination mode, without
Marker samples are come with fluorescent material, it is more easy.
Using surface plasma resonance (SPR) sensor detection testing medium optical property (such as dielectric thickness, refraction
Rate etc.) slight change, its core component is metal function layer, passes through the boundary being present between metal function layer and testing medium
The surface plasma-wave (Surface Plasmon Wave, abbreviation SPW) in face realizes the detection of near interface.Spr sensor leads to
Often by metal function layer and the substrate of the metal function layer is supported to form.Substrate needs to use transparent, smooth material to ensure
SPR phenomenons can be excited and be easy to measure resonance condition, base material also needs to hard and has stronger adhesion with metal, with
Ensure that formed spr sensor has longer service life and long-time stability.Although spr sensor detection is sensitive, have
Hope and replace traditional enzyme linked immunosorbent assay (ELISA) technology (ELISA).But realize that the external optical device of its precise positioning is more stupid
Weight, the popularization of its application is thus limited to a certain extent.
1998, Ebbesen et al. reported the super of the metal film structures that are carved with sub-wavelength array of orifices on Nature
Phenomenon (Extraordinary Optical Transmission, EOT) is transmitted, the light of specific wavelength passes through metal the two-dimentional holes battle array
After array structure, transmitted light intensity is much larger than the result calculated according to classical physics optical theory, and also much larger than as shared by aperture
The result that the area ratio of metal surface is directly calculated.Super transmission phenomenon is the result of Localized field enhancement.Based on superpower light
The plasma sensor of transmission (EOT) can use incoherent light source excitating surface plasma, real with portable spectrometer
Now detect.But the sensitivity of these devices is than traditional spr sensor order of magnitude lower.Had been reported that and reported in the past
Intensity coherent detection is carried out using EOT devices, surface molecular is coupled the reduction (absorptivity for generally causing intensity in transmission in detection
Increase).But this needs the experimental provision of complexity with a large amount of post processings of data to obtain consistent result, because these
Spectral signature also includes skew, and without reference zone.
Utility model content
The utility model provide it is a kind of without frequency conversion cubical array plasma resonance sensor, solve prior art etc. from
Sub-resonance sensor detection sensitivity is limited, and the large-scale not readily portable technical problem of device, realizes hypersensitive, label-free
Biomolecule detection, open offer base for realize the portable medical biology sensor of early detection disease biomarker
Plinth.
To achieve the above object, the utility model proposes one kind without frequency conversion cubical array plasma resonance sensor, bag
Plasma resonance substrate is included, is the array of cavities of nanostructured, covers multi-layered material structure layer thereon, including from bottom to up successively
The first metal layer, insulating barrier and the second metal layer of arrangement, the multi-layered material structure layer formed in substrate be embedded in it is described etc.
Optical resonator array in ion resonance sensor, the optical resonator are the cavity of tapered cups.
Preferably, the cavity depth of the tapered cups is 250~1000nm, the first metal layer thickness is 20~
120nm, thickness of insulating layer 20nm, the second metal layer thickness are 20~120nm.
Preferably, the cavity depth of the tapered cups is 300nm, and the first metal layer thickness is 90nm, insulating barrier
Thickness is 20nm, and the second metal layer thickness is 90nm.
Preferably, the substrate of the plasmon resonance devices is thermoplastic polyester material, and the first metal layer is titanium
Layer, the insulating barrier is cadmium sulfide or silica, and the second metal layer is layer gold.
Preferably, the thermoplastic polyester material is polyethylene terephthalate.
Beneficial effect：
No frequency conversion cubical array plasma resonance sensor provided by the utility model, in three-dimensional taper nanometer cup array etc.
From nanocomposite optical resonant cavity array is embedded in resonance device, the sensor that phasmon-photon based on generation reacts to each other is set
Meter and inducing method.The utility model sensor is realized based on transmission peaks Strength Changes, but resonant wavelength or frequency are without displacement
High-sensitivity detection variations in refractive index.Different from resonance sensor from the past all other grade, the utility model is resonating
Intensity in transmission has lasting, selective change but without the displacement of resonant frequency or wavelength spectrally when spike is long.In addition,
The wave-length coverage of no Strength Changes is also shown, these wave-length coverages can be used as reference zone.The utility model is received this uniqueness
Rice phasmon body nano-cavity device is referred to as multi-layer nano Lycurgus cup array (ML-namoLCA), because lower floor's nanometer cup knot
Structure has similar optical property to the Lycurgus cup that roman makes.By being sensed in high-performance Conventional nano plasma
The array of cavities of nanostructured is added on device, it can be seen that brand-new optics and spectrum property.Especially, on ML-
NanoLCA, the multi-layered material structure layer RI covered during plasma resonance wavelength increase can cause intensity in transmission or formant to carry
The increase taken, but peak wavelength position is not offset.The change for detecting intensity in transmission during by monitoring resonant wavelength is realized.
In addition, the utility model sensor includes a wavelength region not changed with RI change intensities.The utility model exists
A kind of new phasmon RI inducing methods are presented on the basis of being significantly improved to current SPR system.With traditional SPR
Inductor is different, and change of the utility model sensor in the case where being offset without formant by transmiting peak intensity realizes RI
Sensing, therefore, there is no need to the spectroscope with high spectral resolution.
The utility model sensor, which has introduced a kind of RI changes, will not cause peak wavelength shift, but RI changes can lead to
Cross the new phasmon sensing device that high sensitivity changes to detect using peak strength.Only need detection RI vertical incidence
Light, and result is unrelated with polarization.The optical characteristics and bio-sensing result of the utility model sensor are to following medical grade from sharp
First resonance sensing system has great importance.Strength Changes do not occur because intensity changes and had in the range of fixed wave length
Spectral regions, so if light excite it is reasonable in design with optical detection, such as detected simultaneously using dual wavelength incident light, one is being detected
The middle wavelength that Strength Changes occur is used to obtain measurement data, and another does not have the wavelength of Strength Changes to be used as internal reference point,
The utility model sensor has self very high reference ability.It is related to intensity as the ability of the sample for reference of their own
It is special that measurement (being difficult control in the application outside in the measurement, sample is set with sample changed in controlled experiment room) has
Importance.It can be used to detect the small change of any variations in refractive index of unprovoked and the caused intensity of light source for example, referring to area.Thus may be used
See, the utility model sensor make the portable medical biology sensor of early detection disease biomarker be developed into can
Energy.
Brief description of the drawings
Fig. 1 is structural representation of the utility model without frequency conversion cubical array plasma resonance sensor；
Fig. 2 is top view under microscope of the utility model without frequency conversion cubical array plasma resonance sensor；
Fig. 3 is configuration of surface schematic diagram of the utility model without frequency conversion cubical array plasma resonance sensor；
Fig. 4 is cavity structure depth schematic diagram of the utility model without frequency conversion cubical array plasma resonance sensor；
Fig. 5 a are sectional view of the utility model without frequency conversion cubical array plasma resonance sensor；
Fig. 5 b are Fig. 5 a A portions enlarged diagrams；
Fig. 6 is the sensor of only layer of metal layer respectively to air, water, the transmission spectrum of IPA3 kind sample detections；
Fig. 7 is respectively the water (RI=1.33) with air (RI=1), three kinds as covering layer material of IPA (RI=1.37)
The transmission spectrum of senser element；
Fig. 8 is the utility model without testing result of the frequency conversion cubical array plasma resonance sensor using CdS as insulating barrier
Figure；
Fig. 9 be the utility model without frequency conversion cubical array plasma resonance sensor with SiO2For the testing result of insulating barrier
Figure；
Figure 10 is that the utility model is illustrated without spectrum of the frequency conversion cubical array plasma resonance sensor using CdS as insulating barrier
Figure；
Figure 11 be the utility model without frequency conversion cubical array plasma resonance sensor with SiO2Show for the spectrum of insulating barrier
It is intended to；
Figure 12 is intensity in transmission change schematic diagram of the utility model without frequency conversion cubical array plasma resonance sensor；
Figure 13 is the signal that the utility model carries out DNA hybridization detection without frequency conversion cubical array plasma resonance sensor
Figure；
Figure 14 is Figure 13 B portions enlarged drawing；
Figure 15 is that the utility model carries out biotin-streptomysin combination inspection without frequency conversion cubical array plasma resonance sensor
The schematic diagram of survey；
Figure 16 is the biotin of passage over time-strepto- that the intensity in transmission change through the utility model sensor detects
The combination situation schematic diagram of Avidin；
Figure 17 is Figure 16 C portions enlarged drawing；
Figure 18 is the average intensity value comparison diagram of two detection experiments.
In figure：1- plasma resonance substrates；2- the first metal layers；3- insulating barriers；4- second metal layers；5- resonators；M-
Incident light；N- transmitted lights.
Embodiment
To enable above-mentioned purpose of the present utility model, feature and advantage more obvious understandable, below in conjunction with the accompanying drawings and tool
Body embodiment is described in further detail to the utility model.
Embodiment 1
One kind is present embodiments provided without frequency conversion cubical array plasma resonance sensor, referring to Fig. 1, it is shown that its multilayer
Structure and illumination direction, M show incident light, and N show transmitted light；Referring to Fig. 2, the vertical view of display under an electron microscope
Image, referring to Fig. 3, it is shown that the configuration of surface of the present embodiment sensor obtained by AFM scan.The present embodiment sensor bag
Include plasma resonance substrate 1, be nanostructured array of cavities, thereon cover multi-layered material structure layer, including from bottom to up according to
The first metal layer 2, insulating barrier 3 and the second metal layer 4 of secondary arrangement, the multi-layered material structure layer are formed in substrate 1 and are embedded in
The array of optical resonator 4 in the plasma resonance sensor, the optical resonator 4 are the cavity of tapered cups.
Referring to Fig. 4, it is shown that the approximate depth of the present embodiment cycle sensor cavity structure, the cone of this implementation sensor
The cavity depth of shape cup-shaped is 300nm, and the first metal layer thickness is 90nm, thickness of insulating layer 20nm, second gold medal
It is 90nm to belong to thickness degree.
Referring to Fig. 5 a and Fig. 5 b, the sectional view of the present embodiment sensor shot with focused ion beam (FIB) is shown, it is more
Layer material structures layer is high-visible, and the first metal layer is titanium gold layer, and the insulating barrier is cadmium sulfide or silicon dioxide layer, institute
It is layer gold to state second metal layer.The substrate of the plasmon resonance devices is thermoplastic polyester material, preferred heat in the present embodiment
Plasticity polyester material is polyethylene terephthalate.
The present embodiment is prepared by nano-copy moulding technology without frequency conversion cubical array plasma resonance sensor,
In taper nano-pillar die surface, ethylene glycol terephthalate sheet material is uniformly distributed, solidification 30 seconds to 5 points is carried out under ultraviolet light
Clock, the ethylene glycol terephthalate substrate of periodic nanometer hole pattern is formed, the substrate of formation is stripped out from mould,
Titanium is deposited on by the substrate top surface by electron-beam vapor deposition method and taper nano-pillar inner surface forms the first metal layer, is led to
Cross radio frequency sputtering method and cadmium sulfide or silica are deposited on the first metal layer upper surface formation insulating barrier, pass through electron beam
Gold is deposited on the insulating barrier upper surface and forms second metal layer by evaporation, is consequently formed and is embedded in the taper nano-pillar lining
The nanocomposite optical resonator at bottom.Wherein, the mould is that taper nanometer column model is made by photoetching process on quartz material.
Referring to Fig. 6, show that substrate surface only covers the sensor of layer of metal (Au) layer to empty gas and water, isopropanol three
The transmission spectrum of kind different sample detections, referring to Fig. 7, substrate surface is shown respectively with air (RI=1), water (RI=1.33),
Transmission spectrum of the isopropanol (IPA) (RI=1.37) as the senser element of 3 kinds of different samples of covering layer material, the results showed that,
RI constantly increases, and intensity in transmission also increases therewith, if coating does not have insulating barrier, coating RI increase can cause formant
Red shift, however, when coating is sandwich construction, RI increases the increase that can cause intensity, but under 695nm without detection altogether
Shake the skew at peak, show that the present embodiment sensor has sensitivity and the reliability of height.
Detection to the present embodiment transducer sensitivity
The Gary 5G of the transmitted spectrum of the present embodiment sensor and sensitivity measure wave-length coverage in 400nm-800nm
UV-Vis spectrometric instruments measure.Using 0 baseline correction, in this correction, output spectra is normalized by the light source of system.
The sensitivity of the present embodiment sensor is measured by transmiting the relative change of (T) intensity during wavelength corresponding to maximum intensity,
Represented with unit △ %T/RIU.In order to assess the sensitivity of the present embodiment senser element, in the multi-layered material structure layer of covering
On with the addition of the sucrose solutions of various concentrations (in ultra-pure water, proportion concentration is between 0%-60%).Sucrose concentration it is such a
Change changes to 1.44 equivalent to refractive index from 1.33.In order to identify the nanometer insulating barrier being clipped in the middle in multi-layered material structure layer
The influence of the material properties of optical cavity, respectively to CdS and SiO2Sensor as insulating barrier is tested.Such as Fig. 8
It is shown, it is shown that as sucrose solution concentration increases (from 0%-60%), the experimental transmissive using CdS as the sensor of insulating barrier
Spectrum, as shown in Figure 9, it is shown that as sucrose solution concentration increases (from 0%-60%), with SiO2Sensing as insulating barrier
The experimental transmissive spectrum of device, as a result show with optical index RI increase, transmission spectrum resonance peak intensity increase, but it is unglazed
Spectral shift position.
As shown in Figure 10, it is shown that using CdS as the sensor of insulating barrier, be calculated by 3D Fdtd Methods
As sucrose solution concentration increases the transmitted spectrum (from 0%-60%), the simulation result is drawn with the experiment shown in Fig. 8
Collection of illustrative plates coincide very much.As shown in figure 11, it is shown that with SiO2As the sensor of insulating barrier, calculated by 3D Fdtd Methods
Draw as sucrose solution concentration increases transmitted spectrum (from 0%-60%), the simulation result and the reality shown in Fig. 9
Test and show that collection of illustrative plates coincide very much.As shown in figure 12, compared for CdS and SiO2As the sensor of insulating barrier, as sucrose is molten
Liquid concentration and RI increases, the figure of relative transmission intensities change.It is visible in figure, with CdS and SiO2Sensor as insulating barrier
Intensity in transmission trend is similar, is all in rising trend with the increase of sucrose solution concentration, but the two is compared, and is made with CdS
Increase for the sensor intensity in transmission of insulating barrier is relatively small.
Relative change when the sensitivity of the present embodiment sensor passes through resonant wavelength per RI unit (RIU) intensity in transmission come
Calculate, therefore the final unit of sensitivity is △ %T/RIU.During λ=695nm, the sensing using CdS as insulating barrier that calculates
When the sensitivity of device is 660 △ %T/RIU, λ=672nm, calculate with SiO2Sensitivity as the sensor of insulating barrier
It is 340 △ %T/RIU.As can be seen here, the high sensitivity using CdS as the sensor of insulating barrier is in SiO2As insulating barrier
The sensitivity of sensor.Sensitivity is almost doubled.Therefore, the insulating barrier of the utility model sensor preferably using CdS as
Insulating barrier.When the present embodiment calculates, only consideration UV curable polymer matrix, the first metal layer titanium gold layer of bottom, CdS are exhausted
Edge layer, the second metal layer Au layers at top, and water coating.By optimizing CdS thickness of insulating layer and top second metal layer
The thickness of Au layers, the electric-field intensity increase being stored in insulating barrier, while also strengthen with the coupled outside of matrix.
The structure of the present embodiment sensor is surrounded including one by two metal layers, and the Febby- of insulator is used as using CdS
Perrot chambers (optical resonator of Fabry-Perot double-reflecting faces, are called Fabry-Perot chamber).Formed needed for insulating barrier
The thickness for the CdS materials wanted is fixed really, is constructive interference occur after a round trip in insulating barrier.When round trip mutually includes
When the phase of CdS-Au interfaces complex reflection coefficient is multiplied by 2 π equal to an integer, constructive interference just there occurs.If insulating barrier
Phasmon structure and nanocomposite optical resonant cavity are designed to be located at identical resonant wavelength or frequency, when the refraction system of coating
During number change, the change of peak transmission can be neglected, because peak transmission forms local maxima in device geometric aspects.Therefore, in order to obtain
Insulating barrier is designed to slightly offset from resonance by get Geng Gao sensitivity, the present embodiment sensor.
Embodiment 2
Using the utility model DNA hybridization detection is carried out without frequency conversion cubical array plasma resonance sensor.
On single stranded DNA crossover process, the utility model is soaked without frequency conversion cubical array plasma resonance sensor first
Enter in one 10 μM of single stranded DNA (ssDNA) probe solution (DNA-1), this solution by the sulfydryl of DNAs one end come modify from
And DANs is fixed on the Au layers of top the first metal layer.Then the utility model sensor is immersed in 1 μM of confining liquid
In (6- sulfydryl -1- ethanol (MCH)), then it is immersed in 1 μM of DNA-2 (3 ' complementary bases to), hybridization reaction occurs.
Such as Figure 13, it is shown that the transmitted spectrum and the schematic diagram of the process measured after each single stranded DNA hybridization step.Figure
14 be Figure 13 partial enlarged drawing, it is shown that Strength Changes during peak wavelength.
Utilize combination of the utility model without frequency conversion cubical array plasma resonance sensor biotin-Streptavidin
Detection.
Such as Figure 15, it is shown that the transmitted spectrum and the schematic diagram of the process that each biotin-streptomysin measures after combining.
Figure 16 shows the biotin of passage over time-strepto- is affine that the intensity in transmission change through the utility model sensor detects
The combination situation of element.Figure 17 is Figure 16 partial enlarged drawing, shows the combination of biotin-Streptavidin.Figure 18 is with column diagram
Average intensity value when above-mentioned two tests each hybridization step is shown, wherein error bars represent standard deviation.
Intensity in transmission increases to 0.191 ± 0.005% because DNA-1 surface combines from 0.076 ± 0.006%,
Intensity slightly reduces after MCH cultures, is down to 0.189 ± 0.006%.After hybridization reaction is by being immersed in DNA-2 solution, resonance wave
Intensity in transmission increases to 0.203 ± 0.007% to detect when long.
Performance of the utility model sensor in terms of signal to noise ratio need to be important to note that.According to flat spectrum area (400-
425nm) noise intensity that single sample measures is defined as 0.008% by the standard deviation of signal.It can be seen that the intensity of enabling signal
Value is 0.076%, therefore signal to noise ratio is always greater than 95.If signal definition is changed into this practicality newly into minimum detection relative intensity
Type sensor is 0, then signal to noise ratio can be always greater than 1250.It can be seen that the height of the sensitivity of the utility model sensor.
Embodiment 3
The detection of tumor marker CEA concentration
CEA is produced during development of fetus, and CEA generation stops before birth.The normal level of Healthy People is about 3-
5ng/mL.But in the people that body has situation such as to suffer from lung cancer, colon cancer and breast cancer, its concentration has significant increase (＞
10ng/mL)。
The utility model sensor can reach by monitoring the change of peak strength to CEA label-free detection limit (LOD)
1ng/mL(5pM).In the present embodiment, LOD is defined with CEA concentration limit.It is not excluded for the utility model sensor
Actual LOD obtained by when detecting the sample of lower concentration in the sample of detection lower concentration may be than obtained by the present embodiment
Experiment value is lower.ML-nanoLCA sensing capabilities are very outstanding compared with current SPR system.Use commercially available SPR system
During detection, the LOD that as a result shows CEA is 100ng/mL, it is necessary to which LOD is reduced into 3ng/mL using secondary antibody mark.Can
See, the utility model sensor can realize more accurate, sensitive testing result.
The utility model embodiment is described in detail above, specific case used herein is to the utility model
Principle and embodiment be set forth, the explanation of above example be only intended to help understand method of the present utility model and
Its core concept；Meanwhile for those of ordinary skill in the art, according to thought of the present utility model, in embodiment
And there will be changes in application, in summary, this specification content should not be construed as to limitation of the present utility model.
Claims (5)
1. one kind is without frequency conversion cubical array plasma resonance sensor, it is characterised in that is nanometer including plasma resonance substrate
The array of cavities of structure, multi-layered material structure layer, including the first metal layer, the insulating barrier arranged successively from bottom to up are covered thereon
And second metal layer, it is humorous that the multi-layered material structure layer forms the optics being embedded in the plasma resonance sensor in substrate
Shake chamber array, and the optical resonator is the cavity of tapered cups.
2. no frequency conversion cubical array plasma resonance sensor according to claim 1, it is characterised in that the beaker flask
The cavity depth of shape is 250~1000nm, and the first metal layer thickness is 20~120nm, thickness of insulating layer 20nm, described
Second metal layer thickness is 20~120nm.
3. no frequency conversion cubical array plasma resonance sensor according to claim 2, it is characterised in that the beaker flask
The cavity depth of shape is 300nm, and the first metal layer thickness is 90nm, thickness of insulating layer 20nm, the second metal layer
Thickness is 90nm.
4. no frequency conversion cubical array plasma resonance sensor according to any one of claims 1 to 3, it is characterised in that institute
The substrate for stating plasmon resonance devices is thermoplastic polyester material, and the first metal layer is titanium gold layer, and the insulating barrier is sulphur
Cadmium or silica, the second metal layer are layer gold.
5. no frequency conversion cubical array plasma resonance sensor according to claim 4, it is characterised in that the thermoplasticity
Polyester material is polyethylene terephthalate.
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