• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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    • 专利摘要:
    The invention relates to an improved surface plasmon resonance - based hydrogen sensor with an inclined fiber grating surface structure, comprising an ASE broadband light source (1), a polarization controller (2), a single mode fiber (3), and an air chamber base body (4 ), an air inlet (5), an air outlet (6), a fiber optic Pd / Au thin film hydrogen sensor (7), a spectrum analyzer (8) and an air chamber barrier (9), wherein a surface of the fiber optic Pd / Au thin film Hydrogen sensor (7) is coated with an Au nano thin layer and a Pd nano thin layer and a fiber core of the fiber optic Pd / Au thin layer hydrogen sensor (7) is engraved with an inclined fiber Bragg grating.
    公开号:CH715321A2
    申请号:CH00984/19
    申请日:2019-08-05
    公开日:2020-03-13
    发明作者:Shen Changyu；Jin Meng；Gong Jiaqi
    申请人:Univ Jiliang China；
    IPC主号:
    专利说明:

    Technical area
    The present invention proposes an improved surface plasmon resonance-based hydrogen sensor with an inclined fiber-grating surface structure and belongs to the field of fiber sensor technology.
    background
    [0002] Pd is a noble metal with stable chemical properties. Pure Pd has a silvery metallic sheen. Pd can absorb gaseous hydrogen with a volume 900 times that of Pd, with most other gases obviously not being absorbed. Therefore, based on these properties of Pd, Pd can be used as a sensitive material in a hydrogen sensor. When SPR is excited on a surface of a Pd layer or a Pd composite layer, a hydrogen concentration can be measured by monitoring a change in a resonance spectrum of the sensitive layer.
    Compared with an ordinary FBG, a plane of a TFBG grating is no longer perpendicular to an axial direction of an optical fiber but has an inclination angle θ, so that light from a fiber core in a large number of higher order modes guided in the fiber cladding are, can be coupled, which leads to an improvement in the radiation coupling.
    An SPR detection technique has advantages such as real-time performance, high speed, high sensitivity, and feature-free properties. Surface plasmon resonance can easily be excited on the metal Au. Usually, an SPR characteristic of a TFBG modified with an Au thin film is used for detection.
    Summary
    In view of the disadvantages in the prior art, it is an object of the invention to provide an improved surface plasmon resonance-based hydrogen sensor with an inclined fiber grating surface structure. Au and Pd nanoparticles are produced using a chemical liquid phase reduction. The controllable growth of an Au nano thin film and a Pd nano thin film on a quartz substrate is realized by using a technique of molecular self-assembly (SAMs) and a chemical coating method. An Au nano thin film, the thickness of which is approximately 20 nm, is built up on a pretreated inclined Bragg grating by deposition, and then a Pd nano thin film is deposited by using a H2PdCl4 solution having a concentration of 1.25 mmol / l. After the absorption of gaseous hydrogen by the Pd thin layer, palladium hydride is formed and an existing refractive index of the Pd / Au thin layer changes and influences the transmission characteristics of a clad light mode, which causes a change in the transmission spectrum and generates a spectral amplitude curve. An inclined Bragg grating within the layer can generate light which is coupled by a fiber core to a large number of higher order modes that are guided in the fiber cladding, which leads to an improvement in the radiation coupling. In the range of a hydrogen concentration of 1.5% to 4%, the fiber-optic Pd / Au thin-film hydrogen sensor has a good linear response characteristic; for every 1% change in the hydrogen concentration, the change in the spectral amplitude is 0.005 db, so the improved surface plasmon resonance-based hydrogen sensor has a high sensitivity and resolution.
    The present invention is implemented with the following technical solution: An improved surface plasmon resonance-based hydrogen sensor with an inclined fiber grating surface structure of an AES broadband light source (1), a polarization controller (2), a single mode fiber (3) is provided. , an air chamber base body (4), an air inlet (5), an air outlet (6), a fiber optic Pd / Au thin-film hydrogen sensor (7), a spectrum analyzer (8) and an air chamber barrier (9), one surface of the fiber optic Pd / Au thin film hydrogen sensor is coated with an Au nano thin film and a Pd nano thin film; a fiber core of the fiber optic Pd / Au thin film hydrogen sensor (7) is engraved with an inclined fiber Bragg grating (12); a left end of the polarization regulator (2) is connected to the ASE broadband light source (1), a right end of the polarization regulator (2) is connected to a left end of the monomode fiber (3), a right end of the fiber optic Pd / Au thin-film hydrogen sensor (7) is connected to the spectrum analyzer (8), the polarization controller (2) is designed to regulate a polarization state of incident light, with an air inlet flow corresponding to an air inlet flow in an air chamber and being kept stable at a flow rate of 1000 sccm and the test temperature is kept at 23 °.
    The inclined Bragg grating (12) of the fiber optic Pd / Au thin film hydrogen sensor (7) is made of a single mode fiber using a phase matching method and has a grating length of 10 nm, a grating period of 556.6 nm and an inclination angle of 4 °.
    [0008] A wavelength range of the ASE broadband light source (1) is 1420 nm to 1620 nm.
    The modified with an Au nano thin film TFBG has a thickness of 20 nm and a surface on which a structure of an array of gold elements of equilateral triangles is formed by etching to excite a strong surface plasmon resonance, with a thickness of an equilateral triangular Gold element is 10 nm and a side length of the equilateral, triangular gold element is 10 nm and a distance between centers of equilateral, triangular gold elements is 20 nm.
    The Pd nano-thin film is a sensitive material and has a thickness in the range from 5 nm to 100 nm.
    The operation of the present invention is as follows: The polarization controller is designed to regulate the polarization direction of the transmitted light, incident light can be through the fiber-optic Pd / Au thin-film hydrogen sensor (7) with the inclined fiber Bragg grating ( 12) are coupled by the fiber core in a large number of higher order modes that are guided in the fiber cladding, which leads to an improvement in the beam coupling. The inclined grating meets the following phase matching conditions:
    Neff, n <i> eff, core, and n <i> eff, clad each correspond to an existing refractive index of a core mode corresponding to a wavelength λB, an existing refractive index of a core mode corresponding to λ <i> clad and an existing refractive index of a cladding mode i- ter order. and θ are a period of the TFBG and an inclination angle of an inner grating, respectively. Only one wavelength of the cladding mode shifts with a change in an external refractive index, this change being related to a degree of scattering of the cladding mode caused by the external refractive index. When gaseous hydrogen occurs in the vicinity of the Pd thin film, the Pd film is converted into palladium hydride, and this reaction is reversible. According to the optical properties of Pd and PdHx, a dielectric constant of the Pd thin film drops with an increase in the hydrogen concentration, causing the external refractive index to change. Assuming that the change in the external refractive index is Δns, the wavelength shift ΔλB of the Bragg mode and the wavelength shift Δλ <i> clad of the cladding mode are derived as follows:
    The structure of the TFBG was not changed, / ns = 0 and for a typical single mode fiber (e.g. SMF-28), neff / ns = 0 and n <i> eff / ns = 0, and thus
    In the present invention, a Pd nano thin film (11) is used. Pd can absorb gaseous hydrogen which has a volume that is 900 times the volume of Pd, although Pd obviously does not absorb most other gases. Thus, Pd can be used as a sensitive material of a hydrogen sensor. If gaseous hydrogen occurs in the vicinity of a Pd layer, hydrogen molecules (H2) are separated into hydrogen atoms (H), whereby these can then easily diffuse through the Pd layer and ultimately the Pd layer is converted into palladium hydride. This reaction is reversible. According to the optical properties of Pd and PdHx, a dielectric constant of the Pd thin film falls with an increase in the hydrogen concentration, causing a change in the external refractive index.
    In the present invention, the inclined Bragg grating (12) is used, wherein a grating surface of the inclined Bragg grating (12) is no longer perpendicular to an axial direction of an optical fiber but has an inclination angle θ so that light from a The fiber core can be coupled in a large number of higher order modes, guided in the cladding of the fiber, which leads to an improvement in the radiation coupling. For an effect on the external refractive index, only one wavelength of the cladding mode shifts with a change in an external refractive index, this change being related to a degree of scattering of the cladding mode which is caused by the external refractive index. For a temperature response, all resonance wavelengths of the TFBG have the same temperature dependency (with an offset of about 10 pm / ° C each), whereby the cross-influence of all other scanning modes can be eliminated taking into account a relative wavelength shift. For a voltage response, a wavelength shift in the Bragg mode is greater than a wavelength shift in a cladding mode of a higher order.
    Advantageous effects of the present invention are as follows:The Pd nano thin film (11) which has a fairly strong absorption of hydrogen gas is proposed as a sensitive material of a hydrogen sensor, and the sensitivity of the sensor to a change in the concentration of hydrogen is obviously improved. In addition, the radiation coupling is improved by using an inclined Bragg grating TFBG (12). It was found through observation that the sensitivity of the hydrogen sensor was noticeably improved. A new method is therefore provided which is easy to carry out and has high reliability and sensitivity for the detection of hydrogen.
    Brief description of the drawings
    Fig. 1 is a schematic representation of an apparatus of an improved surface plasmon resonance based hydrogen sensor with an inclined fiber grating surface structure in accordance with the present invention; and FIG. 2 is a schematic representation of a structure of an array of gold elements of equilateral triangles on an Au nanoscale, applied to a surface of an improved surface plasmon resonance-based hydrogen sensor with an inclined fiber grating structure according to the present invention.
    Detailed description
    In the following, the present invention will be described with reference to the accompanying drawings using a specific embodiment.
    Referring to Fig. 1, there is provided an improved surface plasmon resonance based hydrogen sensor with an inclined fiber grating surface structure comprising an ASE broadband light source (1), a polarization controller (2), a single mode fiber (3), a Air chamber base body (4), an air inlet (5), an air outlet (6), a fiber-optic Pd / Au thin-film hydrogen sensor (7), a spectrum analyzer (8) and an air chamber barrier (9), with an Au nanodin-film ( 10) and a Pd nano thin film (11) are applied to a surface of the fiber optic Pd / Au thin film hydrogen sensor (7); a thickness of the Au nano thin film (10) is 20 nm; a surface of the Au nanoscale is etched so that it forms an array of equilateral, triangular gold elements to excite a strong surface plasmon resonance, a thickness of an equilateral, triangular gold element being 10 nm and a side length of the equilateral, triangular gold element being 10 nm and a distance between centers of equilateral, triangular gold elements is 20 nm; wherein the thickness of the Pd nano thin film is in the range of 5 nm to 100 nm; wherein a fiber core of the fiber optic Pd / Au thin film hydrogen sensor (7) is engraved with an inclined Bragg grating (12) and the inclined Bragg grating (12) has a length of 10 nm, a grating period of 556.6 nm and an inclination angle of 4 °, wherein a left end of the polarization controller (2) is connected to the ASE broadband light source (1), a right end of the polarization controller (2) is connected to a left end of the single mode fiber (3) and a right end of the fiber optic hydrogen sensor (7) is connected to the spectrum analyzer (8).
    The Au nano thin film and the Pd nano thin film are arranged on the surface of the Pd / Au thin film fiber optic hydrogen sensor. First, a layer of Au nano thin film is formed on a surface of an optical fiber, then a Pd thin film is formed on a surface of the Au thin film by deposition. The specific steps are sequentially as follows: TFBG surface cleaning, surface hydroxylation, self-assembly of a coupling reagent APTMS as a monomolecular layer, absorption of Au nanoparticles, creation of an Au thin layer and building this Au thin layer, the thickness of which is approximately 20 nm, on a surface of a pretreated TFBG by deposition. The deposition time is 15 minutes and the coating solution has a temperature of 23 ° C. The Pd nano-thin layer is then applied using an H2PdCl4 solution with a concentration of 1.25 mmol / l and finally a coated sensor is packed for protection.
    权利要求:
    Claims (1)
    [1]
    1. An improved surface plasmon resonance-based hydrogen sensor with an inclined fiber grating surface structure, comprising an ASE broadband light source (1), a polarization controller (2), a monomode fiber (3), an air chamber base body (4), an air inlet (5) , an air outlet (6), a fiber optic Pd / Au thin film hydrogen sensor (7), a spectrum analyzer (8) and an air chamber barrier (9), a surface of the fiber optic Pd / Au thin film hydrogen sensor (7) having an Au Nano thin layer (10) and a Pd nano thin layer (11) is coated; wherein a thickness of the Au nano-thin film (10) is 20 nm; a surface of the Au nano-thin layer (10) is etched in the form of an array of gold elements from equilateral triangles to produce a strong surface plasmon resonance, wherein a thickness of a triangular, equilateral gold element is 10 nm, one side length of the triangular, equilateral gold element is 10 nm and one Distance between centers of equilateral triangular gold elements is 20 nm; a thickness of the Pd nano-thin film is in the range of 5 nm to 100 nm; a fiber core of the Pd / Au fiber optic thin film hydrogen sensor (7) is engraved with an inclined Bragg grating (12), the inclined Bragg grating (12) has a length of 10 nm, a grating period of 556.6 nm and one Tilt angle of 4 °; a left end of the polarization controller (2) is connected to the ASE broadband light source, a right end of the polarization filter is connected to a left end of the single mode fiber (3); a right end of the fiber optic Pd / Au thin film hydrogen sensor (7) is connected to the spectrum analyzer.
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    同族专利:
    公开号 | 公开日
    CN109060728A|2018-12-21|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    CN110286090B|2019-04-19|2021-12-07|武汉理工大学|Optical fiber hydrogen sensor based on Au @ Pd nanoparticles and preparation method and application thereof|
    CN110261351A|2019-06-03|2019-09-20|暨南大学|Plasma resonance inclined optical fiber grating hydrogen gas sensor, detection system and method|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    CN201811059808.1A|CN109060728A|2018-09-12|2018-09-12|Inclined optical fiber grating surface superstructure enhances surface plasma resonance hydrogen sensor|
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