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WO2009109065A1 - Capteur par résonance plasmonique de surface couplé à un guide d'ondes, dispositif de détection de capteur et procédé de détection de ce capteur - Google Patents

Capteur par résonance plasmonique de surface couplé à un guide d'ondes, dispositif de détection de capteur et procédé de détection de ce capteur Download PDF

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Publication number
WO2009109065A1
WO2009109065A1 PCT/CN2008/000437 CN2008000437W WO2009109065A1 WO 2009109065 A1 WO2009109065 A1 WO 2009109065A1 CN 2008000437 W CN2008000437 W CN 2008000437W WO 2009109065 A1 WO2009109065 A1 WO 2009109065A1
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WIPO (PCT)
Prior art keywords
layer
sensor
light source
refractive index
dielectric waveguide
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PCT/CN2008/000437
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English (en)
Chinese (zh)
Inventor
郑铮
赵欣
朱劲松
范江峰
Original Assignee
国家纳米科学中心
北京航空航天大学
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Publication date
Application filed by 国家纳米科学中心, 北京航空航天大学 filed Critical 国家纳米科学中心
Priority to PCT/CN2008/000437 priority Critical patent/WO2009109065A1/fr
Publication of WO2009109065A1 publication Critical patent/WO2009109065A1/fr

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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
    • G01N21/55—Specular reflectivity
    • G01N21/552—Attenuated total reflection
    • G01N21/553—Attenuated total reflection and using surface plasmons

Definitions

  • the present invention relates to the field of sensors and sensing technologies, and in particular to a surface plasmon resonance sensor having a fast response, a sensing detecting device and a detecting method thereof. Background technique
  • SPR Surface Plasmon Resonance
  • ATR At Tenua ted Tota Ref ect ion
  • the wave vector of the surface plasma matches the wave vector of the SPR evanescent wave, and the reflected light energy becomes smaller than that of the total reflection, and the incident light energy Coupled into the surface plasma waves, resulting in a significant reduction in reflected light energy.
  • This particular angle of incidence is called the surface plasmon resonance angle.
  • surface plasmon resonance angle By angular scanning, surface plasmon resonance peaks (ie, minimum reflection intensity values) can appear on the reflection spectrum.
  • the refractive index of the medium in contact with the metal surface is different, the surface plasmon resonance angle is different. By measuring the position of the surface plasmon resonance angle and the change in its reflected light intensity, some characteristic parameters of the medium near the metal surface and the amount of change thereof can be obtained.
  • Waveguide Coup ed Surface P lasmon Resonance is an SPR resonance mode. And Bioelectronics, 2004, vo l 20, p633-642 ). Compared with the traditional SPR detection method, the WCSPR detection method can achieve higher sensitivity, larger signal-to-noise ratio and wider dynamic measurement range.
  • the sensor structure for realizing WCSPR detection is mainly composed of a first metal layer, a dielectric waveguide layer, a second metal layer and a detected layer. Measurement.
  • the most commonly used SPR scan mode has a kind of ': ⁇
  • Angle scanning method (Angu lar Interroga t ion ): This is the most common scanning method for traditional SPR detection.
  • the method can use a fixed-wavelength light source to rotate the SPR detection structure or the incident light source by a mechanical device to change the incident angle of the incident light at the interface of the SPR detection structure to find the SPR resonance angle.
  • the running speed of the rotating table is limited, so the scanning speed of the system is slow, and it is difficult to achieve fast real-time measurement with high time resolution, and the mechanical scanning device is also disadvantageous for system miniaturization and high-throughput detection.
  • This method can also be used Focus the beam, not the near-plane beam that is typically used, as the incident light.
  • the focused beam is composed of plane waves of different wave vectors, so that it is possible to cover a certain range of incident angles without changing the central incident angle.
  • the method can be performed by using a spatial photodetector array device
  • the detection speed is relatively fast, but the speed of the detected array electronics can only reach a level of tens of kHz.
  • Wavelength Interrogation This method is to change the wavelength of incident light when the angle of incidence is fixed, or to input a wide-spectrum light source to measure the response of light incident at different wavelengths. The corresponding light wavelength of the SPR resonance.
  • the cost of achieving high resolution is very expensive, the volume of the device is difficult to reduce, and the scanning speed is limited.
  • Intensity trajectory method This method detects the change of the characteristics of the substance to be tested by measuring the change of the reflected light intensity when the incident angle is fixed and the incident wavelength and power are fixed. The intensity scanning method is faster, but its resolution is very low.
  • the object of the present invention is to overcome the drawbacks of the slow detection speed of the conventional WCSPR sensing technology, thereby providing a WCSPR sensor device that can be quickly scanned and detected.
  • Another object of the present invention is to provide a detecting device using the above WCSPR sensor.
  • a waveguide coupling surface plasmon resonance sensor comprising a dielectric waveguide layer, wherein the material of the dielectric waveguide layer is a nonlinear optical material.
  • the nonlinear optical material is preferably a third-order nonlinear optical material, such as carbon nanotubes, diarylferrocene, phthalocyanine, porphyrin, polydiacetylene, polyaniline, polythiophene, polypyrrole, polyphenylacetylene, poly A third-order nonlinear optical material composed of one or more of acrylonitrile, a 4, 4'-bipyridine metal complex or an azobenzene polymer.
  • a third-order nonlinear optical material such as carbon nanotubes, diarylferrocene, phthalocyanine, porphyrin, polydiacetylene, polyaniline, polythiophene, polypyrrole, polyphenylacetylene, poly
  • a third-order nonlinear optical material composed of one or more of acrylonitrile, a 4, 4'-bipyridine metal complex or an azobenzene polymer.
  • the thickness of the dielectric waveguide layer is preferably less than 100 ⁇ m, and in particular, the thickness of the dielectric waveguide layer is more preferably in the range of 1 ⁇ m - 10 ⁇ m.
  • at least a cladding layer is disposed on both sides of the dielectric waveguide layer, and a refractive index of the cladding layer should be smaller than a refractive index of the dielectric waveguide layer.
  • the material of the cladding layer may preferably be an optical glass, a polymer, an optical crystal or a metal or the like.
  • the present invention provides a waveguide coupled surface plasmon resonance sensing measuring apparatus comprising the above sensor and a control light source for varying the refractive index of the dielectric waveguide layer.
  • the control light source is preferably a laser light source and/or a pulse light source.
  • the pulsed light source it is particularly preferable that the sum of the rising edge and the falling edge width of the waveform of the output pulse light is larger than fifty percent of the pulse width.
  • the waveform of the pulse light output pulse light is preferably a triangular type, a Gaussian type or a hyperbolic tangent type.
  • the pulse light source preferably outputs a pulse light source whose amplitude of the pulse light is adjustable.
  • the above-mentioned sensor measuring device further includes a light detecting device for detecting the output light of the detecting light source reflected by the sensor, wherein the light detecting device can complete the output detecting light during one pulse period of the pulse light source At least one measurement, such as a photodetector, a light-like oscilloscope, or a CCD.
  • a light detecting device for detecting the output light of the detecting light source reflected by the sensor, wherein the light detecting device can complete the output detecting light during one pulse period of the pulse light source At least one measurement, such as a photodetector, a light-like oscilloscope, or a CCD.
  • the present invention provides a sensing method for the above-described waveguide coupled surface plasmon resonance sensing measuring device, comprising the following steps:
  • step (c) further comprises the step of adjusting the intensity of the control light output by the control light source.
  • the step (d) comprises: firstly, according to the waveform information recorded by the photodetector, combined with the optical nonlinear characteristics of the material used in the sensor dielectric waveguide layer, the dielectric waveguide layer corresponding to the waveguide coupling formant is obtained. Refractive index; Then, the refractive index and/or thickness variation of the detected layer is obtained by the waveguide coupling formant and its corresponding dielectric waveguide layer refractive index.
  • the invention has the following advantages: Ultra-fast all-optical tuning for ultra-high-speed WCSPR scanning with scan speeds that are orders of magnitude higher than existing SPR scanning methods.
  • the invention is based on the third-order nonlinear effect caused by the pulse light source. For short pulses with a certain repetition frequency, each pulse can be subjected to SPR detection, and the scanning time depends on the width of the light pulse.
  • the pulse width generated by the existing pulse light source can reach the order of several tens of femtoseconds or picoseconds, so that the SPR signal can be scanned in a very short time.
  • the present invention can be used to monitor physical, chemical or biological processes in real time, and obtain process information with extremely high time resolution.
  • the time to perform a scan is the time-domain width of a pulse. Since the time-domain width of the pulse can be very narrow and can reach the order of femtoseconds, the scanning speed can be very fast, so that continuous scanning of the ultra-fast reaction process can be realized.
  • the entire reaction process can be monitored on a fine time axis to obtain process information such as accurate kinetic curves.
  • the invention can be used to monitor rapid biochemical reaction processes. SPR sensor components are mostly used for biochemical detection, and dynamic monitoring of biochemical reaction processes to obtain biodynamic information is one of the most significant applications. However, due to the limitation of scanning speed, the existing SPR sensing system is difficult to dynamically monitor the reaction process for some biochemical reactions with short reaction times (on the order of seconds or less). The invention can greatly improve the time resolution on the time axis of the kinetic curve and dynamically monitor the reaction mechanism of the rapid biochemical reaction.
  • FIG. 1 is the basic structure of an ultrafast all-optical tuned WCSPR sensor chip. 1 is the first metal layer, 2 is the dielectric waveguide layer, 3 is the second metal layer, 4 is the detected layer, 5 is the fluid layer, and 6 is the base layer.
  • Figure 2 shows the sensor structure for plasmon resonance of an ultrafast all-optical waveguide coupled surface.
  • Figure 3 is a schematic diagram of an ultrafast all-optical tuned WCSPR sensing system.
  • Figure 4 is a graph showing the change in the intensity of reflected light over time in the case of changing the refractive index of the measured layer.
  • Figure 5 is a graph showing the relationship between the two lowest point spacings of the time and intensity curves of the detected light reflection signal and the refractive index of the measured layer.
  • Figure 6 is a graph showing the change in reflectance of light with the refractive index of the dielectric waveguide layer.
  • the present invention adopts a waveguide-coupled surface plasmon resonance structure as a basic structure of a sensor, and modulates the WCSPR response of the detection light by tuning optical characteristics of the dielectric waveguide layer (such as refractive index) to obtain a sample to be detected. Information to achieve rapid detection of the sample being tested.
  • the WCSPR structure shown in Figure 1 contains a multi-layer structure.
  • the surface plasmon resonance wave vector generated at the interface between the second metal layer 103 and the layer to be detected 104 is affected by the waveguide mode characteristics of the dielectric waveguide layer 102. Since surface plasmon resonance can only be excited by the TM mode of incident light, the TM mode reflection at the interface between dielectric waveguide layer 102 and second metal layer 103 can be expressed as:
  • ⁇ k ⁇ k represents the z-direction component of the wave vector in the i-th layer, represents the z-direction component of the wave vector in the k-th layer, represents the dielectric constant of the material of the k-th layer, and represents the dielectric constant of the material of the i-th layer, theoretically
  • the reflectivity equation can be expressed as:
  • phase of the reflected light can be expressed as:
  • the reflectivity; r x , Struktur indicates the incident light incident from the first waveguide layer, the reflection from the second to n-th waveguide layers, and the reflection coefficient back to the first waveguide layer; indicating the n-1th waveguide
  • the invention adopts a material having a third-order nonlinear optical effect as an optical medium layer material in the WCSPR sensing structure, and the optical physical property parameters such as the refractive index of the material may change with the electromagnetic field intensity of the incident light.
  • materials having a third-order nonlinear optical effect are exemplified.
  • the third-order nonlinear optical effect originates from the third-order polarization rate, and the electromagnetic field of the light can cause the refractive index of the third-order nonlinear optical material to change, that is, the refractive index effect related to the light intensity.
  • the refractive index of a material having a third-order nonlinear optical effect can be expressed as:
  • Re represents the real part
  • ⁇ is the part of the fourth-order tensor of the third-order polarization rate 3) that contributes to the change in refractive index.
  • Equation (5) shows that there is a linear correspondence between the refractive index change of the third-order nonlinear material and the magnitude of the light intensity and the third-order nonlinear coefficient of the material. Therefore, by changing the intensity of the tuned light, the refractive index of the dielectric waveguide layer can be modulated, thereby changing the WCSPR resonance condition of the detected light in the WCSPR sensor, and realizing WCSPR modulation.
  • a third-order nonlinear optical waveguide material with a third-order nonlinear optical coefficient of 1.87 X l can be obtained using a doped polymer (Proc. SPIE 2693, 523-531, 1996).
  • the already well-developed planar optical waveguide processing method can be fabricated into the waveguide structure required by the invention.
  • the short-light pulse generation technology mainly includes two kinds of Q-switching technology and mode-locking technology.
  • a pulsed laser with pulse width ⁇ 1 ps, peak power > 10 kW, repetition rate >10 GHz and time jitter ⁇ 10 f s can be achieved using mode-locking technology.
  • a precise phase encoding in the frequency domain can be achieved by means of gratings, spatial phase modulators, fiber gratings, etc., to achieve pulse shape control in the time domain (IEEE J. Quantum E. tron., 1992, vol. 28, pp. 908 920) .
  • the sensor structure shown in FIG. 1 is composed of a multilayer film, which is a transparent base layer 106, a first metal layer 101, a dielectric waveguide layer 102, a second metal layer 103, and a detected layer 104, from top to bottom.
  • the material of the dielectric waveguide layer 102 uses a nonlinear optical material, particularly a third-order nonlinear optical material such as carbon nanotubes, diarylferrocene, phthalocyanine, guanidine, polydiacetylene, polyaniline, polythiophene, Polypyrrole, polyphenylacetylene, polyacrylonitrile, 4, 4'-bipyridine metal complex or azobenzene polymer, etc.
  • the thickness of the dielectric waveguide layer 102 should be greater than the wavelength of the detection light, which is less than ⁇ ⁇ ⁇ ⁇ , and particularly preferably, the range is ⁇ ⁇ ⁇ - 10 ⁇ ⁇ .
  • the ligand layer 104 contains a ligand, which can be affected by the solution to be tested. The body reacts to change the properties of the layer to be detected 104 such that its thickness or refractive index changes.
  • both sensors comprise a base layer 206, a first metal layer 201, a dielectric waveguide layer 202, a second metal layer 203 and a detected layer 204, in addition, Figures 2a and 2b A cladding layer 207 is also provided, and the cladding layer 207 may be disposed only on both sides of the dielectric waveguide layer 202 (as shown in FIG.
  • the cladding layer 207 functions to control the pulsed laser light that is coupled into the dielectric waveguide layer 202 by the end face to propagate in the dielectric waveguide layer 202.
  • the material of the cladding layer 207 can be selected, for example, optically. Glass, polymer, optical crystal or metal, etc., but whose refractive index should be less than the refractive index of the dielectric waveguide layer material.
  • Fig. 3 is a schematic structural view of a waveguide coupled surface plasmon resonance sensing measuring device.
  • the chip structure of the sensor is the same as that of FIG. 2b. 761.
  • the refractive index of the 980 nm incident light is 1. 7761.
  • the first metal layer 307 and the second metal layer 309 are made of pure gold and have a thickness of 20 nm.
  • PthPC third-order nonlinear material 2, 9, 16, 23-tetrakis(phenylthio)- 29 ⁇ , 31 ⁇ -phthalocyanine
  • the cladding (not shown in Figure 3) material is also pure gold and is prepared by mask evaporation.
  • the detected layer 313 was covalently attached to the IgG molecule with 16-mercaptohexadecylcarboxylic acid as a biochemical modification to a thickness of about 3 nm.
  • the WCSPR sensing detecting device in this embodiment further includes a control light source 301, a detecting light source 302 and a photodetector 312.
  • the scanning and variation of the control light intensity can modulate the refractive index of the dielectric waveguide layer, thereby realizing the medium.
  • the scanning and tuning of the refractive index of the waveguide layer is within a certain range. Since the frequency of the pulsed light source can reach above 10 GHz in the prior art, high-speed scanning is truly realized.
  • the sum of the rising edge and the falling edge width of the pulsed light source output pulse waveform is preferably greater than 50% of the pulse width, so that the refractive index of the dielectric waveguide layer changes relatively gently during one pulse period, and thus, the photodetector 312 There is sufficient response time to detect a change in intensity of the detection light, and the pulse waveform may preferably be a conventional pulse waveform such as a triangle, a Gaussian type or a hyperbolic tangent type.
  • the amplitude of the pulse light source is adjustable, and the variation range of the refractive index of the dielectric waveguide layer can be adjusted by adjusting the amplitude.
  • a light detecting device having a high detecting speed such as a photodetector, an optical sampling oscilloscope or a CCD, should be used to complete at least one measurement of the outputted detection light in one pulse period.
  • the output wavelength of the control light source 301 is 1550 nm, and the output waveform is a Gaussian pulse having a half-height width of 10 ps, a repetition frequency of 10 GHz, and a peak power of 520 mW.
  • the detection source 302 is a stable narrow-band monochromatic light source. In this example, a 980 nm semiconductor infrared laser source is used, and the average output power is 10 mW.
  • a filter 303 and a polarizing plate 304 for changing the detected light into P polarization are also provided on the output light path of the detecting light source.
  • the photodetector 312 uses a semiconductor ultra-high speed photodetector with a bandwidth of 40 GHz, and the detection area is preferably larger than the reflected spot area, and may be equal to or smaller than the reflected spot area according to actual needs.
  • the coupling optical element for detecting light incidence may be a semi-cylindrical prism or a 45760° right-angle prism.
  • a 45° right-angle prism is selected, and the glass material of the prism material is ZF7, and the refractive index corresponding to the incident light of 980 nm is 1. 7761.
  • the detection cell 31 0 of the WCSPR sensing measuring device shown in Fig. 3 is prepared from a transparent polydithiosilane PDMS material, and is bonded to the detecting chip through silica gel.
  • a) detecting light output from the light source is P-polarized, coupled into the glass substrate layer 306 by the prism 305, and the detected light is reflected by the sensor, and then measured by the photodetector system 311 to adjust the incident angle until the photodetector is used.
  • a waveguide coupling resonance peak can be detected;
  • test solution (mouse ant i-I gG in PBS buffer solution) into the detection cell 310 through a microfluidic syringe pump at a rate of 10 ⁇ ! 7 ⁇ in; when the antibody is detected in the solution ant i- IgG molecule After being combined with the modified human IgG molecule on the detected layer 31 3 , the refractive index of the detected layer 31 3 is changed; the coupling resonance angle of the sensor is changed, and the waveguide coupling resonance peak received by the photodetector moves or disappears;
  • the data processing system can obtain the refractive index of the dielectric waveguide layer when the waveguide coupling resonance occurs according to the time domain waveform and the detected light intensity recorded by the photodetector in the above steps a) to c), and those skilled in the art utilize these Parameters, according to the matching formula or calibration coefficient composed of Fresnel equation, can obtain the refractive index and / or thickness change of the detected layer, combined with the sample conditions and other information, and then can obtain human IgG and mouse ant i-IgG molecules Identify kinetic related data.
  • the refractive index of the dielectric waveguide layer varies with the instantaneous intensity of the control light pulse.
  • the range of the refractive index scan of the dielectric waveguide layer can be controlled according to actual needs. If the detected layer is combined with the acceptor in the sample to be tested, the refractive index of the detected layer changes too much. Large, so that the detector can not receive the waveguide coupling formant, you can try to increase the amplitude of the control source output pulse, and expand the refractive index scanning range of the dielectric waveguide layer.
  • the control light source of the embodiment uses a pulse light source
  • the light pulse is equivalent to repeatedly adjusting the intensity of the output light of the control light source in the amplitude range during the ascending and descending process
  • the refractive index of the dielectric waveguide layer is repeatedly changed to ensure
  • the photodetector can still detect the waveguide coupling formant
  • the data processing system can obtain the change of the refractive index of the dielectric waveguide layer according to the control light intensity corresponding to the re-detection of the waveguide coupling formant, thereby knowing the refraction of the detected layer.
  • Changes in the rate and/or thickness and those skilled in the art, in conjunction with information such as sample conditions, can provide data on the molecular recognition kinetics of human IgG and mouse ant i-IgG.
  • Fig. 4 is a graph showing the relative reflectance of the detection light under control light tuning as a function of time when the refractive indices of the detected layers are 1.459, 1.464 and 1.469, respectively. It can be seen from the figure that as the refractive index of the detected layer changes, the position of the resonance absorption peak also changes, and the larger the refractive index of the detected layer, the larger the time interval between the plasmon resonance peaks of the two surfaces.
  • Figure 5 shows the time interval between the refractive index of the detected layer and the surface plasmon resonance peak. It can be seen from the figure that as the refractive index of the detected layer increases, the time interval of the surface plasmon resonance absorption peak increases.
  • Fig. 6 is a graph showing the relationship between the reflectance (intensity) of the detected light and the refractive index of the dielectric waveguide layer measured by the apparatus shown in Fig. 3 when the refractive index of the detected layer is 1.464. From this curve, it was found that the refractive index of the dielectric waveguide layer corresponding to the plasmon resonance peak of the waveguide coupling surface under the structural condition of the present embodiment was 1.716.
  • each of FIG. 4 The pulse laser intensity corresponding to each moment is known, and according to formula (5), the time axis of the abscissa can be converted into the corresponding dielectric waveguide layer refractive index, which is actually FIG.

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Abstract

L'invention concerne un capteur par résonance plasmonique de surface couplé à un guide d'ondes qui peut balayer et détecter rapidement, un dispositif de mesure de capteur et un procédé de détection de ce capteur. Une couche de guide d'ondes diélectrique (102) du capteur est réalisée en un matériau optique non linéaire.
PCT/CN2008/000437 2008-03-05 2008-03-05 Capteur par résonance plasmonique de surface couplé à un guide d'ondes, dispositif de détection de capteur et procédé de détection de ce capteur WO2009109065A1 (fr)

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PCT/CN2008/000437 WO2009109065A1 (fr) 2008-03-05 2008-03-05 Capteur par résonance plasmonique de surface couplé à un guide d'ondes, dispositif de détection de capteur et procédé de détection de ce capteur

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PCT/CN2008/000437 WO2009109065A1 (fr) 2008-03-05 2008-03-05 Capteur par résonance plasmonique de surface couplé à un guide d'ondes, dispositif de détection de capteur et procédé de détection de ce capteur

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN102262073A (zh) * 2011-04-14 2011-11-30 北京航空航天大学 一种基于波导耦合表面等离子共振的降低背景影响的检测方法
CN102495508A (zh) * 2011-12-21 2012-06-13 中国计量学院 太赫兹波高速开关装置及其方法
CN111272713A (zh) * 2020-03-24 2020-06-12 聊城大学 一种侧激发Kretschmann型波导SPR传感器的制备方法
CN112525859A (zh) * 2020-10-19 2021-03-19 中国科学院微电子研究所 表面等离激元共振传感测量方法、装置及系统

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102262073A (zh) * 2011-04-14 2011-11-30 北京航空航天大学 一种基于波导耦合表面等离子共振的降低背景影响的检测方法
CN102495508A (zh) * 2011-12-21 2012-06-13 中国计量学院 太赫兹波高速开关装置及其方法
CN111272713A (zh) * 2020-03-24 2020-06-12 聊城大学 一种侧激发Kretschmann型波导SPR传感器的制备方法
CN112525859A (zh) * 2020-10-19 2021-03-19 中国科学院微电子研究所 表面等离激元共振传感测量方法、装置及系统
CN112525859B (zh) * 2020-10-19 2022-07-01 中国科学院微电子研究所 表面等离激元共振传感测量方法、装置及系统

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