CN115219422B - A broadband tunable optical fiber surface plasmon sensing probe - Google Patents
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- G01N21/55—Specular reflectivity
- G01N21/552—Attenuated total reflection
- G01N21/553—Attenuated total reflection and using surface plasmons
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Abstract
本发明属于微纳光子学及光纤传感技术领域，提出了一种宽带可调谐的光纤表面等离激元传感探针，利用光学胶将三层的光栅耦合结构集成到光纤端面上。在光栅衍射的作用下，入射光可以在金属膜的内表面和外表面分别激发出表面等离激元，使反射谱中出现两个共振峰，利用反射谱中的两个共振峰飘移可以分别实现对生物分子和超声波的检测。该传感器的优势在于，通过改变纳米光栅的周期，两个反射共振峰的位置可以在可见光和近红外范围内连续调谐，这突破了传统光纤表面等离激元激发波长难以扩展到近红外波长的问题，在生物检测、化学分析、以及超声波检测等方面有着广泛的应用前景。
The present invention belongs to the field of micro-nano photonics and optical fiber sensing technology, and proposes a broadband tunable optical fiber surface plasmon sensing probe, which uses optical glue to integrate a three-layer grating coupling structure onto the end face of the optical fiber. Under the action of grating diffraction, the incident light can excite surface plasmons on the inner and outer surfaces of the metal film respectively, so that two resonance peaks appear in the reflection spectrum. The drift of the two resonance peaks in the reflection spectrum can respectively realize the detection of biological molecules and ultrasound. The advantage of this sensor is that by changing the period of the nano grating, the positions of the two reflection resonance peaks can be continuously tuned in the visible light and near-infrared range, which breaks through the problem that the traditional optical fiber surface plasmon excitation wavelength is difficult to extend to the near-infrared wavelength, and has broad application prospects in biological detection, chemical analysis, and ultrasonic detection.
Description
Technical Field
The invention relates to the technical fields of micro-nano photonics and optical fiber sensing, in particular to a broadband tunable optical fiber surface plasmon sensing probe.
Background
Compared with the traditional detection technology, the surface plasmon resonance (Surface Plasmon Resonance, SPR) detection technology has the advantages of high sensitivity, strong anti-interference capability, no marking, real-time detection and the like, and has wide application prospects in the fields of life science, medical detection, food detection and the like. However, the current commercial SPR detection systems are generally prismatic SPR sensors, which are generally large in size and complex in system, and do not meet the current pursuit of miniaturization and portability, and are shown in Hlubina, P, et al Spectrum interferometry-based surface plasmon resonance sensor. The optical fiber type SPR sensor has the advantages of miniaturization, remote sensing and the like, can overcome the limitations and can be widely studied, is one of the most developed detection technologies at the present stage, and particularly see Micheletto R,et al.Modeling and test of fiber-optics fast SPR sensor forbiological investigation.Bosch M E,et al.Recent development in optical fiber biosensors.Yao Y,et al.Surface plasmon resonance biosensors and its application., in order to adapt the sensor to detection under various environments, a plurality of methods for tuning resonance wavelengths in spectrums, such as changing materials, film thicknesses, shapes, structures, sizes and the like of nano structures, have been proposed.
At present, research on optical fiber type SPR sensors is mostly focused on the side surface of an optical fiber, and detection of external environments, such as inclined fiber Bragg gratings (TFBG), is realized by exciting gold film surface plasmons (Surface Plasmons, SPs) on the side surface of the optical fiber, which is shown in Caucheteur C,et al.Ultrasensitive plasmonic sensing in air using optical fibre spectral combs.Wang R,et al.Operando monitoring of ion activities in aqueous batteries with plasmonic fiber-optic sensors. in detail, but the resonance wavelength of a traditional SPR optical fiber sensor is difficult to tune continuously, and the requirement on the angle of incident light is high, so that the functions of biochemical detection and the like can be realized only in a visible light band generally. In addition, the integration of SPR devices at the fiber end allows for small amounts of sample to be inserted, as opposed to sensors integrated into the fiber side walls, and the signal read directly through dip-and-read, which greatly reduces the difficulty of operation. Therefore, the design of the structure which can effectively and continuously tune the SPs excitation wavelength on the end face of the optical fiber and break through the working wave band to the near infrared or mid infrared region has very important significance.
The invention combines the detection advantages of the optical fiber SPR sensor and the grating diffraction principle to design the broadband tunable optical fiber surface plasmon sensing probe, and the resonance wavelength of the broadband tunable optical fiber surface plasmon sensing probe can be continuously tuned and can be used for various different application scenes.
Disclosure of Invention
The invention aims to provide a broadband tunable optical fiber surface plasmon sensing probe which can be used for high-sensitivity biochemical detection and ultrasonic detection and is a novel SPR optical fiber sensor structure. According to the invention, the diffraction effect of the grating is utilized, so that the vertically incident light beam generates an inclination angle and excites the surface plasmon between the metal film and the object to be detected, and the detection of the refractive index change of the object to be detected is realized. The technology can realize the regulation and control of resonance wavelength in a wide spectrum range, has the advantages of high sensitivity, quick response time and the like, and has wide application prospects in the fields of biochemical detection and the like.
The technical scheme of the invention is as follows:
The broadband tunable optical fiber surface plasmon sensing probe has tunable resonant wavelength and two resonant modes, and the two resonant modes correspond to two application scenes respectively, namely high-sensitivity label-free biochemical detection and high-sensitivity ultrasonic detection;
The broadband tunable fiber surface plasmon sensing probe comprises an optical fiber and a grating coupling structure, wherein the grating coupling structure is fixed on the end face of the optical fiber through optical cement, and the detection of an object to be detected is realized by exciting SPs in the grating coupling structure. The designed structure mainly comprises three layers, namely a grating, a dielectric medium and a metal film from bottom to top, wherein the grating is in contact fixation with an optical cement, and the metal film is in contact with a solution to be tested;
Based on the principle of grating diffraction, incident light with short wavelength is obliquely incident into a dielectric medium at a first-order diffraction angle after passing through the grating, and incident light with long wavelength forms evanescent waves at the interface of the grating and the dielectric medium;
When the wave vector matching condition is met, the incident light with short wavelength excites surface plasmons at the contact surface of the metal film and the solution to be detected, the surface plasmons are the first resonance mode of the broadband tunable optical fiber surface plasmon sensing probe, the incident light with long wavelength excites the surface plasmons at the contact surface of the metal film and the dielectric medium, the surface plasmons are the second resonance mode of the broadband tunable optical fiber surface plasmon sensing probe, different short wavelength resonance peaks are generated by different refractive indexes of the solution to be detected in the first resonance mode, detection of an object to be detected is achieved, the refractive index of the optical adhesive is changed due to the action of ultrasonic waves in the second resonance mode, and the long wavelength resonance peaks drift, so that detection of the ultrasonic waves is achieved.
The light beam is vertically incident to the grating.
The period of the grating is determined according to the target resonance wavelength. In addition, the incident light with a certain wavelength range can lead the light beam to generate a first-order diffraction angle only, and the influence of high-order diffraction is ignored. Based on the principle of grating diffraction, the position of the formants can be continuously tuned from the visible light band to the near infrared region.
The wave vector matching condition is that when the light beams all meetWhen the broadband tunable optical fiber surface plasmon sensing probe has the first resonance mode, all the light beams meetThe broadband tunable optical fiber surface plasmon sensing probe has only the second resonance mode when the optical beam exists inAnd the wavelength of (2) is again presentWherein lambda is the wavelength of the beam, p is the period of the grating, and n 2 is the refractive index of the dielectric.
The optical fiber is a single-mode optical fiber or a multi-mode optical fiber.
The grating is manufactured by a micro-nano processing technology or a template transfer method, the grating material is metal, the grating period determines the working wave band of the broadband tunable fiber surface plasmon sensing probe, and when a specific resonance wavelength is needed, the corresponding grating period is obtained by combining a grating diffraction formula and a wave vector matching equation.
The resonance mode extends from visible light to the near infrared and mid-infrared bands.
After passing through the grating, the light beam is obliquely incident into the dielectric medium at a first-order diffraction angle, and evanescent waves are generated at the interface of the dielectric medium and the metal film. The evanescent wave has certain penetrability and can penetrate through a relatively thin metal film. When no surface plasmon resonance occurs, the evanescent wave is almost completely reflected back. When the wave vector of the evanescent wave is equal to that of the surface plasmon at the interface of the metal film and the object to be detected, SPR phenomenon can occur, and the energy of the evanescent wave is transferred to SPs, so that the reflectivity at the resonance wavelength is reduced, and a resonance peak appears in the reflection spectrum. When the refractive index of the object to be detected is increased, the resonance peak can be subjected to red shift, so that the change of the refractive index of the object to be detected is detected. This is the first mode of the sensor, which has a shorter resonant wavelength.
In addition to the formants produced by the first mode, there is a longer wavelength formant in the reflection spectrum, which is caused by the second mode. The larger the wavelength, the larger the corresponding first order diffraction angle, when the grating period is fixed. The incident light with short wavelength has a first order diffraction angle smaller than 90 degrees, and is obliquely incident into the dielectric medium at the first order diffraction angle, and is in a first mode. Whereas incident light of long wavelength corresponds to a first order diffraction angle of 90 degrees or more, which results in an evanescent wave of the incident light at the interface of the grating and the dielectric. When the wave vector matching condition is satisfied, the evanescent wave excites SPs on the inner surface of the metal film, resulting in the appearance of long wavelength formants. There are two distinct formants in the reflectance spectrum. In addition, the optical cement is a flexible material, and changes in refractive index occur due to the action of ultrasonic waves, resulting in shift of resonance peak of long wavelength. With the increase of the refractive index of the optical cement, the resonance peak with long wavelength can generate a red shift phenomenon, thereby realizing the detection of ultrasonic waves.
When the wavelength is fixed, the first order diffraction angle is inversely proportional to the period of the grating, and the first order diffraction angle is related to the resonant wavelength, so the period of the grating can determine the resonant wavelength. The specific formula is shown below.
pn2sin(θ)=mλ (1)
k0n2sin(θ)＝kspp (2)
Formula (1) is a grating diffraction formula, p is the period of the grating, θ is the diffraction angle, n 2 is the refractive index of the dielectric medium, λ is the wavelength of incident light, m is the diffraction order, when the minimum wavelength of the broadband incident light satisfiesWhen we need only consider first order diffraction. Equation (2) is a wave vector matching equation, and k spp and k 0 represent a surface plasmon wave vector and an incident light wave vector, respectively. Combining equation (1) and equation (2) can be obtained:
Where ε m represents the dielectric constant of the metal and ε d represents the dielectric constant of the solution to be tested. As shown in formula (3), a specific resonant wavelength corresponds to a specific grating period, and the formants can be continuously tuned in the sensor by processing a grating coupling structure with a specific period and fixing the grating coupling structure to the end face of the optical fiber through optical cement.
Analysis of the variables in equation (3) shows that the resonant wavelength of the first mode is independent of the refractive index of the optical cement. In addition, the resonance wavelength of the second mode is also independent of the refractive index of the solution to be measured. Thus, the two modes can coexist and do not affect each other. By analyzing the structure calculated by the numerical value, the short wavelength resonance peak in the reflection spectrum can drift when the refractive index of the object to be detected changes, but the resonance peak with long wavelength can be stable, and the short wavelength resonance peak in the reflection spectrum can be stable and the resonance peak with long wavelength can drift when the dielectric medium or the optical refractive index changes. This is quite consistent with the theoretical analysis results, indicating that the sensor has the advantage of multifunctional detection.
Compared with the prior art, the optical fiber sensor has the advantages that firstly, the grating coupling structure is combined with the optical fiber, the resonance wavelength of the sensor can be continuously tuned by controlling the period of the grating, secondly, two application scenes exist in the sensor, the interference between the two application scenes is small, the sensor can be used for high-sensitivity biochemical detection and high-sensitivity ultrasonic detection at the same time, thirdly, the sensor can expand the working wavelength from visible light to near infrared and middle infrared bands, and fourthly, the sensitivity of the sensor has good polarization angle tolerance.
Drawings
FIG. 1 is a block diagram of a broadband tunable fiber surface plasmon sensing probe;
FIG. 2 is a schematic diagram of a first mode for detecting a solution to be tested;
FIG. 3 is a schematic diagram of a second mode for detecting ultrasound;
FIG. 4 shows the refractive index of the solution to be measured, and the reflection spectrum without ultrasonic waves, wherein the refractive index of the ultraviolet optical cement is unchanged;
FIG. 5 is a reflection spectrum of a solution to be measured with the presence of ultrasonic waves and with the refractive index unchanged, at which time the refractive index of the ultraviolet optical cement is changed.
Detailed Description
In order that those skilled in the art will better understand the present application, a technical solution in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in which it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, shall fall within the scope of the application.
In this example, a gold film is selected as the outermost metal film, siO 2 is used as the dielectric, gold is used as the material of the grating, and an ultraviolet curable adhesive is selected to fix the grating structure to the end face of the optical fiber. As shown in formula (3), the position of the short wavelength formant corresponds to a specific grating period, and the resonance wavelength is selected by setting the specific grating period. Taking a sensor with a resonance wavelength of 1550nm as an example, the period of the grating was calculated to be 1153nm by analysis of equation (3).
The specific process for designing the optical fiber sensor mainly comprises the steps of firstly taking a clean silicon wafer as a substrate, plating 25nm of gold, 220nm of SiO 2 and 10nm of gold on the silicon wafer in sequence by utilizing a magnetron sputtering coating instrument, secondly etching a grating with a period of 1153nm, a width of 300nm and a depth of 10nm on an outer gold film by utilizing a Focused Ion Beam (FIB), thirdly coating an ultraviolet curing adhesive on the end face of the optical fiber, fourthly contacting the end face of the optical fiber with the grating coupling structure, curing the ultraviolet curing adhesive by irradiation of an ultraviolet lamp, and fifthly separating the optical fiber from the silicon wafer, wherein the grating coupling structure on the silicon wafer is completely transferred onto the end face of the optical fiber due to weak bonding force between the gold and the silicon substrate, so that the preparation of the sensor is completed. When the wavelength range of the incident light is from 1400nm to 2000nm, two modes exist in the sensor, so that the detection of the solution to be detected and the ultrasonic wave is realized.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The broadband tunable optical fiber surface plasmon sensing probe is characterized in that the resonance wavelength of the broadband tunable optical fiber surface plasmon sensing probe is provided with two resonance modes, and the two resonance modes respectively correspond to two different application scenes, namely high-sensitivity label-free biochemical detection and high-sensitivity ultrasonic detection;
The broadband tunable fiber surface plasmon sensing probe comprises an optical fiber and a grating coupling structure, wherein the grating coupling structure is fixed on the end face of the optical fiber through optical cement;
The optical fiber is characterized in that a light beam is emitted from an optical fiber core and enters an optical adhesive to be contacted with a grating, and based on the principle of grating diffraction, the incident light with short wavelength is obliquely incident into a dielectric medium at a first-order diffraction angle after passing through the grating, and an evanescent wave is generated at the interface of the dielectric medium and a metal film;
The wave vector matching condition is that when the light beams all meet When the broadband tunable optical fiber surface plasmon sensing probe has the first resonance mode, all the light beams meetThe broadband tunable optical fiber surface plasmon sensing probe has only the second resonance mode when the optical beam exists inAnd the wavelength of (2) is again presentWherein lambda is the wavelength of the light beam, p is the period of the grating, and n 2 is the refractive index of the dielectric medium;
When the wave vector matching condition is met, the incident light with short wavelength excites surface plasmons at the contact surface of the metal film and the solution to be detected, the surface plasmons are the first resonance mode of the broadband tunable optical fiber surface plasmon sensing probe, the incident light with long wavelength excites the surface plasmons at the contact surface of the metal film and the dielectric medium, the surface plasmons are the second resonance mode of the broadband tunable optical fiber surface plasmon sensing probe, different short wavelength resonance peaks are generated by different refractive indexes of the solution to be detected in the first resonance mode, detection of an object to be detected is achieved, the refractive index of the optical adhesive is changed due to the action of ultrasonic waves in the second resonance mode, and the long wavelength resonance peaks drift, so that detection of the ultrasonic waves is achieved.
2. The broadband tunable fiber surface plasmon sensing probe of claim 1 wherein said light beam is normally incident at the grating.
3. The broadband tunable fiber surface plasmon sensing probe of claim 1 or 2, wherein the period of said grating is determined according to a target resonance wavelength.
4. The broadband tunable optical fiber surface plasmon sensing probe of claim 1 wherein said optical fiber is selected from a single mode optical fiber or a multimode optical fiber.
5. The broadband tunable optical fiber surface plasmon sensing probe according to claim 1, wherein the grating is manufactured by a micro-nano processing technology or a template transfer method, the grating material is metal, the grating period determines the working band of the broadband tunable optical fiber surface plasmon sensing probe, and when a specific resonance wavelength is required, the corresponding grating period is given by combining a grating diffraction formula and a wave vector matching formula.
6. The broadband tunable fiber surface plasmon sensing probe of claim 1 wherein said resonance mode extends from visible light to near infrared and mid infrared bands.
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