CN107807110B - SPR sensor-based solution concentration detection system and preparation method of SPR sensor - Google Patents
SPR sensor-based solution concentration detection system and preparation method of SPR sensor Download PDFInfo
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- CN107807110B CN107807110B CN201710893394.1A CN201710893394A CN107807110B CN 107807110 B CN107807110 B CN 107807110B CN 201710893394 A CN201710893394 A CN 201710893394A CN 107807110 B CN107807110 B CN 107807110B
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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
- G01N21/59—Transmissivity
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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
- G01N21/59—Transmissivity
- G01N2021/5903—Transmissivity using surface plasmon resonance [SPR], e.g. extraordinary optical transmission [EOT]
Abstract
The invention discloses a solution concentration detection system based on an SPR sensor, which comprises an SPR sensor, a broadband light source, a sample cell, an optical fiber spectrometer and a computer, wherein the SPR sensor is arranged in the sample cell, an input optical fiber and an output optical fiber are respectively arranged at the input end and the output end of the SPR sensor, the input optical fiber is connected with the broadband light source, the output optical fiber is connected with the optical fiber spectrometer, and the optical fiber spectrometer is connected with the computer through a data line; the SPR sensor comprises a detection optical fiber and an asymmetric metal film layer arranged on the detection optical fiber, the detection optical fiber comprises a single-mode optical fiber and multimode optical fibers arranged at two ends of the single-mode optical fiber in a bilateral symmetry mode, and the two multimode optical fibers are connected with the single-mode optical fiber through fusion welding.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a solution concentration detection system based on an SPR sensor and a preparation method of the SPR sensor.
Background
Optical Surface Plasmon Resonance (SPR) is an optical physical phenomenon. When a beam of P-polarized light is incident on the prism end face within a certain angle range, surface plasmon waves are generated at the interface between the prism and the metal thin film (Au or Ag). When the propagation constant of the incident light wave matches the propagation constant of the surface plasmon wave, free electrons in the metal film are caused to resonate, i.e., surface plasmon resonance. During analysis, a layer of biomolecule recognition membrane is fixed on the surface of a sensing chip, then a sample to be detected flows on the surface of the chip, if molecules capable of interacting with the biomolecule recognition membrane on the surface of the chip exist in the sample, the refractive index of the surface of the gold membrane changes, and finally SPR angle changes are caused, and information such as the concentration, affinity, kinetic constant, specificity and the like of an analyte is obtained by detecting the SPR angle changes.
Today's SPR sensors are of both prism coupling and fiber coupling types. In prism coupling, total reflection must be generated at a prism-metal interface in order to generate SPR, optical fiber transmission is based on total reflection, and an optical fiber coupling SPR sensor can be designed by using an optical fiber instead of a prism. The core part of the optical fiber SPR sensor is an optical fiber coated with a layer of metal film, and the coating part needs to be removed in advance to expose a fiber core. When the light is totally reflected at the fiber core-metal interface, evanescent waves are generated, and then SPR is generated. The properties of evanescent waves are related to the wavelength of transmitted light, the numerical aperture of optical fibers and the metal material. In the optical fiber SPR, an SPR effect is generated every time total reflection of light occurs. The incident planes of each total reflection in the optical fiber are not completely the same, so that the difference between S polarized light and P polarized light can be disregarded, i.e. no polarizer is needed. The optical fiber has a special structure, and although the sensitivity of an SPR sensor using the optical fiber as a carrier is inferior to that of a prism coupling structure, the optical fiber SPR has the advantages of miniaturization and long-distance transmission. The discovery of surface plasmon resonance has enabled us to have new methods for the measurement of refractive index in liquids, particularly refractive index measurements in turbid liquids. The refractive index is necessarily related to a plurality of physical quantities, for example, the concentration of a plurality of solutions is linearly related to the refractive index, so that a sensing system of the concentration of the solution can be manufactured by SPR.
In the traditional SPR sensor manufacturing process, when the uniform coating on the side surface of the optical fiber requires evaporation coating, the optical fiber can rotate above an evaporation source at a constant speed, the rotation speed is high, the evaporation speed of a film material is reduced as much as possible, and thus uniform coating can be realized. Therefore, the requirement on equipment is high, the current is controlled to be slowly increased in the coating process, the time is long, and the measuring range is limited.
Disclosure of Invention
In order to overcome the defects of the technology, the invention provides a solution concentration detection system based on an SPR sensor and a preparation method of the SPR sensor.
The invention discloses a solution concentration detection system based on an SPR sensor, which comprises the SPR sensor, a broadband light source, a sample cell, an optical fiber spectrometer and a computer, wherein the SPR sensor is arranged in the sample cell, an input optical fiber and an output optical fiber are respectively arranged at the input end and the output end of the SPR sensor, the input optical fiber is connected with the broadband light source, the output optical fiber is connected with the optical fiber spectrometer, and the optical fiber spectrometer is connected with the computer through a data line; the SPR sensor comprises a detection optical fiber and an asymmetric metal film layer arranged on the detection optical fiber, the detection optical fiber comprises a single-mode optical fiber and multimode optical fibers arranged at two ends of the single-mode optical fiber in a bilateral symmetry mode, and the two multimode optical fibers are connected with the single-mode optical fiber through fusion welding.
The preparation method of the SPR sensor comprises the following specific steps:
1) removing the coating layers of a single mode fiber and two multi-mode fibers, wiping the coating layers with alcohol-dipped dust-free cloth, cutting the end face to be smooth, and welding the cut end face by using a welding machine to form a multi-mode-single-mode structure detection fiber;
2) cleaning the beaker by using cleaning powder, and then washing by using deionized water;
3) putting the washed beaker into a drying blast box until the surface of the beaker is free of moisture, closing the blast box, and taking out the beaker after the beaker is cooled;
4) weighing required metal silver and detection optical fibers, putting the metal silver and the detection optical fibers into two beakers separately, and pouring acetone to submerge the silver and the detection optical fibers;
5) putting the two beakers into an ultrasonic cleaning machine for cleaning for 15 minutes, taking out silver from acetone, and drying the detection optical fiber by using nitrogen;
6) turning on a compressor and introducing cooling water;
7) slowly opening an inflation valve, opening an upper cover of the vacuum chamber after the vacuum chamber is filled with air, placing metal silver, and detecting whether the vacuum chamber is a passage or not by using a universal meter;
8) placing the single-mode optical fiber in the detection optical fiber right above the evaporation source;
9) closing the inflation valve, opening a mechanical pump switch, and slowly opening a side pumping valve, wherein the standard that no vibration is sensed is adopted;
10) when the pressure in the vacuum chamber is lower than 10Pa, opening a front-stage valve switch, when the pressure in the vacuum chamber is lower than 5Pa, opening a molecular pump switch, quickly closing a side pumping valve, and quickly opening a gate valve;
11) when the vacuum degree is lower than the vacuum degree, a heating power supply is turned on, the current is slowly adjusted, and the current is stopped to be increased when the heating power is observed to be 150W;
12) after 10 minutes, reducing the current to 0, and turning off the heating power supply;
13) after 60 minutes, cooling the system, turning off the power supply of the molecular pump, turning off the gate valve, and sequentially turning off the power supply of the front valve, the mechanical pump, the main power supply and the cooling water compressor when the rotating speed is about 0;
14) opening an inflation valve, opening an upper cover to take out the optical fiber after the pressure in the vacuum chamber is the same as the pressure of the external environment, and observing the film coating condition;
15) closing the upper cover and the inflation valve of the vacuum chamber, and pumping the vacuum chamber to 300Pa by using a mechanical pump for storage.
The invention has the beneficial effects that:
because light generated by a broadband light source in the device enters the SPR sensor through optical fiber coupling, when light waves meeting resonance conditions excite a metal film to generate Surface Plasma Waves (SPW), a resonance valley is formed in a transmission spectrum, the transmission spectrum is collected and recorded by an optical fiber spectrometer, samples with different refractive indexes are placed in a sample cell, the position of the resonance valley can be moved, and the sensing characteristics of the sensor on the refractive indexes can be calibrated by recording the resonance spectrums of a series of samples. Because the refractive indexes of the liquids or solutions with different concentrations are different, the concentration of the solution can be measured by using the system;
in the invention, the adopted asymmetric coating only needs to keep the welded detection optical fiber above the evaporation source without rotation in terms of manufacturing process, thus having low requirement on equipment and short coating time; from the performance of the sensor, the optical fiber SPR with the asymmetric coating has the thickness from 0 to 30nm, and according to the SPR excitation principle, one resonance absorption peak is excited at a certain metal film thickness, and when a plurality of film thicknesses exist in a section of detection optical fiber, a plurality of resonance absorption peaks are excited, so that the measurement range of the SPR sensor is widened.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the invention, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a schematic diagram of a SPR sensor based solution concentration detection system according to the present invention;
FIG. 2 is a schematic diagram of the structure of a detection fiber in an SPR sensor;
FIG. 3 is a schematic cross-sectional view of the optical fiber of FIG. 2 after being coated with a coating film.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.
Any feature disclosed in this specification (including any accompanying claims, abstract and drawings), may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
As shown in fig. 1 to 3, a solution concentration detection system based on an SPR sensor of the apparatus of the present invention includes an SPR sensor 6, a broadband light source 1, a sample cell 3, a fiber spectrometer 4 and a computer 5, wherein the SPR sensor 6 is installed in the sample cell 3, an input end and an output end of the SPR sensor 6 are respectively installed with an input fiber 21 and an output fiber 22, the input fiber 21 is connected to the broadband light source 1, the output fiber 22 is connected to the fiber spectrometer 4, and the fiber spectrometer 4 is connected to the computer 5 through a data line; the SPR sensor 6 comprises a detection optical fiber and an asymmetric metal film layer 63 arranged on the detection optical fiber, wherein the detection optical fiber comprises a single-mode optical fiber 62 and multimode optical fibers 61 which are arranged at two ends of the single-mode optical fiber 62 in a bilateral symmetry mode.
The preparation method of the SPR sensor comprises the following specific steps:
1) removing the coating layers of a single mode fiber 62 and two multi-mode fibers 61, wiping the coating layers clean by alcohol dipping dust-free cloth, cutting the end face to be smooth, and welding the cut end face by using a welding machine to form a multi-mode-single-mode structure detection fiber;
2) cleaning the beaker by using cleaning powder, and then washing by using deionized water;
3) putting the washed beaker into a drying blast box until the surface of the beaker is free of moisture, closing the blast box, and taking out the beaker after the beaker is cooled;
4) weighing required metal silver and detection optical fibers, putting the metal silver and the detection optical fibers into two beakers separately, and pouring acetone to submerge the silver and the detection optical fibers;
5) putting the two beakers into an ultrasonic cleaning machine for cleaning for 15 minutes, taking out silver from acetone, and drying the detection optical fiber by using nitrogen;
6) turning on a compressor and introducing cooling water;
7) slowly opening an inflation valve, opening an upper cover of the vacuum chamber after the vacuum chamber is filled with air, placing metal silver, and detecting whether the vacuum chamber is a passage or not by using a universal meter;
8) placing the single-mode optical fiber 62 in the detection optical fiber right above the evaporation source;
9) closing the inflation valve, opening a mechanical pump switch, and slowly opening a side pumping valve, wherein the standard that no vibration is sensed is adopted;
10) when the pressure in the vacuum chamber is lower than 10Pa, opening a front-stage valve switch, when the pressure in the vacuum chamber is lower than 5Pa, opening a molecular pump switch, quickly closing a side pumping valve, and quickly opening a gate valve;
11) when the vacuum degree is lower than the vacuum degree, a heating power supply is turned on, the current is slowly adjusted, and the current is stopped to be increased when the heating power is observed to be 150W;
12) after 10 minutes, reducing the current to 0, and turning off the heating power supply;
13) after 60 minutes, the system is cooled, the power supply of the molecular pump is turned off, and the gate valve is turned off; when the rotating speed is to be 0, sequentially closing the power supply of the front-stage valve, the mechanical pump, the main power supply and the cooling water compressor;
14) opening an inflation valve, opening an upper cover to take out the optical fiber after the pressure in the vacuum chamber is the same as the pressure of the external environment, and observing the film coating condition;
15) closing the upper cover and the inflation valve of the vacuum chamber, and pumping the vacuum chamber to 300Pa by using a mechanical pump for storage.
The invention has the beneficial effects that: because light generated by a broadband light source in the device enters the SPR sensor through optical fiber coupling, when light waves meeting resonance conditions excite a metal film to generate Surface Plasma Waves (SPW), a resonance valley is formed in a transmission spectrum, the transmission spectrum is collected and recorded by an optical fiber spectrometer, samples with different refractive indexes are placed in a sample cell, the position of the resonance valley can be moved, and the sensing characteristics of the sensor on the refractive indexes can be calibrated by recording the resonance spectrums of a series of samples. Because the refractive indexes of the liquids or solutions with different concentrations are different, the concentration of the solution can be measured by using the system;
in the invention, the adopted asymmetric coating only needs to keep the welded detection optical fiber above the evaporation source without rotation in terms of manufacturing process, thus having low requirement on equipment and short coating time; from the performance of the sensor, the optical fiber SPR with the asymmetric coating has the thickness from 0 to 30nm, and according to the SPR excitation principle, one resonance absorption peak is excited at a certain metal film thickness, and when a plurality of film thicknesses exist in a section of detection optical fiber, a plurality of resonance absorption peaks are excited, so that the measurement range of the SPR sensor is widened.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (2)
1. The utility model provides a solution concentration detecting system based on SPR sensor, includes SPR sensor, broadband light source, sample cell, fiber optic spectrometer and computer, its characterized in that: the SPR sensor is arranged in the sample cell, an input optical fiber and an output optical fiber are respectively arranged at the input end and the output end of the SPR sensor, the input optical fiber is connected with the broadband light source, the output optical fiber is connected with the optical fiber spectrometer, and the optical fiber spectrometer is connected with the computer through a data line; the SPR sensor comprises a detection optical fiber and an asymmetric metal film layer arranged on the detection optical fiber, the detection optical fiber comprises a single-mode optical fiber and multimode optical fibers arranged at two ends of the single-mode optical fiber in a bilateral symmetry mode, and the two multimode optical fibers are connected with the single-mode optical fiber through fusion welding.
2. A preparation method of an SPR sensor comprises the following specific steps:
1) removing the coating layers of a single mode fiber and two multi-mode fibers, wiping the coating layers with alcohol-dipped dust-free cloth, cutting the end face to be smooth, and welding the cut end face by using a welding machine to form a multi-mode-single-mode structure detection fiber;
2) cleaning the beaker by using cleaning powder, and then washing by using deionized water;
3) putting the washed beaker into a drying blast box until the surface of the beaker is free of moisture, closing the blast box, and taking out the beaker after the beaker is cooled;
4) weighing required metal silver and detection optical fibers, putting the metal silver and the detection optical fibers into two beakers separately, and pouring acetone to submerge the silver and the detection optical fibers;
5) putting the two beakers into an ultrasonic cleaning machine for cleaning for 15 minutes, taking out silver from acetone, and drying the detection optical fiber by using nitrogen;
6) turning on a compressor and introducing cooling water;
7) slowly opening an inflation valve, opening an upper cover of the vacuum chamber after the vacuum chamber is filled with air, placing metal silver, and detecting whether the vacuum chamber is a passage or not by using a universal meter;
8) placing the single-mode optical fiber in the detection optical fiber right above the evaporation source;
9) closing the inflation valve, opening a mechanical pump switch, and slowly opening a side pumping valve, wherein the standard that no vibration is sensed is adopted;
10) when the pressure in the vacuum chamber is lower than 10Pa, opening a front-stage valve switch, when the pressure in the vacuum chamber is lower than 5Pa, opening a molecular pump switch, quickly closing a side pumping valve, and quickly opening a gate valve;
11) when the vacuum degree is lower than the vacuum degree, a heating power supply is turned on, the current is slowly adjusted, and the current is stopped to be increased when the heating power is observed to be 150W;
12) after 10 minutes, reducing the current to 0, and turning off the heating power supply;
13) after 60 minutes, cooling the system, turning off the power supply of the molecular pump, turning off the gate valve, and sequentially turning off the power supply of the front valve, the mechanical pump, the main power supply and the cooling water compressor when the rotating speed is about 0;
14) opening an inflation valve, opening an upper cover to take out the optical fiber after the pressure in the vacuum chamber is the same as the pressure of the external environment, and observing the film coating condition;
15) closing the upper cover and the inflation valve of the vacuum chamber, and pumping the vacuum chamber to 300Pa by using a mechanical pump for storage.
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| US6870237B1 (en) * | 2003-08-26 | 2005-03-22 | National Taiwan University | Repeated structure of nanometer thin films with symmetric or asymmetric configuration for SPR signal modulation |
| CN103900991A (en) * | 2013-12-17 | 2014-07-02 | 中国计量学院 | Refractive index sensor based on surface plasmon resonance |
| CN205317669U (en) * | 2016-01-13 | 2016-06-15 | 中国计量学院 | Hydrogen sensing device based on side is thrown and is ground gradient index fiber |
| CN105866070A (en) * | 2016-05-27 | 2016-08-17 | 哈尔滨工程大学 | Distributed liquid refractive index sensing device based on optical fiber surface plasma resonance |
| CN106017724A (en) * | 2016-05-05 | 2016-10-12 | 北京交通大学 | Liquid-filled D-type hollow core double-cladding optical fiber SPR temperature sensor |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US6870237B1 (en) * | 2003-08-26 | 2005-03-22 | National Taiwan University | Repeated structure of nanometer thin films with symmetric or asymmetric configuration for SPR signal modulation |
| CN103900991A (en) * | 2013-12-17 | 2014-07-02 | 中国计量学院 | Refractive index sensor based on surface plasmon resonance |
| CN205317669U (en) * | 2016-01-13 | 2016-06-15 | 中国计量学院 | Hydrogen sensing device based on side is thrown and is ground gradient index fiber |
| CN106017724A (en) * | 2016-05-05 | 2016-10-12 | 北京交通大学 | Liquid-filled D-type hollow core double-cladding optical fiber SPR temperature sensor |
| CN105866070A (en) * | 2016-05-27 | 2016-08-17 | 哈尔滨工程大学 | Distributed liquid refractive index sensing device based on optical fiber surface plasma resonance |
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