CN215812409U - LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO and sensor thereof - Google Patents
LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO and sensor thereof Download PDFInfo
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Abstract
An LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO and a sensor thereof belong to the field of optical fiber sensors. The LRSPR high-sensitivity optical fiber sensor based on Au-Ag-GO comprises an optical fiber sensing unit, a light source, a spectrometer and a PC which are matched with the optical fiber sensing unit; the optical fiber sensing unit comprises an optical fiber core with an optical fiber cladding removed, and a first optical fiber and a second optical fiber which are respectively connected with two ends of the optical fiber core with the optical fiber cladding removed, wherein a matching layer and an Au-Ag-GO composite material layer are sequentially arranged on the periphery of the optical fiber core with the optical fiber cladding removed from the inner side to the outer side. Due to the application of the Au-Ag-GO composite material layer, the sensitivity of the optical fiber sensor is improved, the surface electric field intensity of the optical fiber sensor is enhanced due to the arranged matching layer, the penetration depth is increased, the performance of the sensor is further improved, and the detection capability can be extended to the detection level of macromolecular cells.
Description
Technical Field
The utility model relates to the technical field of optical fiber sensors, in particular to an LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO and a sensor thereof.
Background
Optical fibers have gradually come into the sight of people as an excellent low-loss transmission line, and sensor research based on optical fibers as waveguides is also being widely and deeply conducted. The optical fiber sensor has many advantages which the traditional sensor does not have, such as magnetic interference resistance, electric insulation, good explosion-proof performance, corrosion resistance, good light guide performance, multi-parameter measurement, small volume, embeddability and the like.
In the field of biological research, a Surface Plasmon Resonance (SPR) sensing method can realize real-time online monitoring of an interaction process of biomolecules, and has the advantages of quick response and no need of labeling. The SPR based on the optical fiber structure is prepared by plating a metal film with a nanometer thickness on the surface of the treated optical fiber. When incident light with a certain specific wavelength irradiates the metal film, the light wave resonates with plasma waves generated on the surface of the metal, so that the energy of the reflected light is sharply reduced to form a resonant trough, the resonant trough is sensitive to the refractive index of the external environment, and the refractive index of the external environment is detected by detecting the movement of the resonant trough. Thus, the research on the application of the sensor based on the fiber SPR effect has been greatly developed. According to previous researches, the sensor based on the fiber SPR effect has high sensitivity and resolution, and is far higher than the sensor of a mode interference type. However, if the analyte is a biological macromolecule such as protein, the size of the biological macromolecule is far higher than the penetration depth of the surface plasmon polariton, which means that the ordinary SPR sensor cannot effectively detect the refractive index change inside the biological macromolecule; on the other hand, the silver film which is often used also has the defect of easy oxidative deterioration, and the service life of the sensor is limited.
LRSPR is an SPR mode excited by adding a matching layer with a lower refractive index than the fiber core between the surface of the fiber core and a metal layer on the basis of a conventional SPR film structure. In recent years, in order to improve the sensitivity and resolution of detection results, the research of sensors based on the long-range surface plasmon mode has attracted continuous attention, and has achieved important research results. For example, a Teflon-AF1600 film is used as a matching layer and a gold film is used as a sensing layer, and a high-sensitivity surface plasmon sensor (Slavik R, Homola J. ultra high resolution long range surface plasmon-based sensor [ J ]. Sensors and Actuators B-Chemical,2007,123(1):10-12.) is designed. Ultra-high resolution long-range surface plasmon biosensors (Shi H, Liu Z, Wang X, et al. A systematic optical waveguide based surface plasmon resonance system [ J ]. Sensors and Actuators B Chemical,2013,185(8): 91-96.) have also been successfully fabricated, but their sensitivity is low and they are not suitable for molecular or cellular scale bio-field monitoring, severely limiting their development.
Graphene Oxide (GO) serving as an important derivative of a graphene-based material shows excellent physical, chemical, optical and electrical properties, is a novel carbon material with excellent performance, has a high specific surface area and good conductivity, and is applied to many fields.
SUMMERY OF THE UTILITY MODEL
According to the problems in the prior art, the utility model discloses an LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO and a sensor thereof.
In order to achieve the purpose, the utility model adopts the following technical scheme:
the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO comprises an optical fiber core with an optical fiber cladding removed, wherein one end of the optical fiber core with the optical fiber cladding removed is connected with a first optical fiber, the other end of the optical fiber core with the optical fiber cladding removed is connected with a second optical fiber, and a matching layer and an Au-Ag-GO composite material layer are sequentially arranged on the periphery of the optical fiber core with the optical fiber cladding removed from the outer side.
Furthermore, the diameter of the fiber core of the optical fiber without the fiber cladding is 200-300 μm, the diameters of the fiber cores of the first optical fiber and the second optical fiber are the same as the diameter of the fiber core of the optical fiber without the fiber cladding, and the fiber cores of the optical fibers are coaxial; the fiber cladding of the first optical fiber is equal to that of the second optical fiber, and the thickness of the fiber cladding of the first optical fiber is 20-30 mu m.
Further, the length of the fiber core of the optical fiber with the cladding removed is 2cm, the length of the first optical fiber is 5cm, and the length of the second optical fiber is 5 cm.
Further, the matching layer is a fluorine-containing complex of terbium (III), and the thickness of the matching layer is 100-110 nm;
the molecular structural formula is as follows:
further, the Au-Ag-GO composite material layer is an Au-Ag-GO uniform mixture layer, and the mass ratio of Au: ag: GO ═ 5:1: 5.
The thickness of the Au-Ag-GO composite material layer is 40-50 nm.
An LRSPR high-sensitivity optical fiber sensor based on Au-Ag-GO comprises the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO, a light source, a spectrometer and a PC; the light source is arranged at the input end of the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO, the output end of the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO is connected with the spectrometer, and the spectrometer is connected with the PC.
The wavelength range of the spectrum is 500-800 nm;
the wavelength range of the spectrometer is 200-1100 nm.
An LRSPR high-sensitivity optical fiber sensor based on Au-Ag-GO has the following detection sensitivity: 9600-12000 nm/RIU.
Compared with the prior art, the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO and the sensor thereof have the beneficial effects that:
according to the LRSPR high-sensitivity optical fiber sensor based on Au-Ag-GO, the design of the Au-Ag-GO composite material layer is adopted, and the advantage that gold is stable in chemical property and not easy to oxidize is utilized, so that the sensor has high sensitivity; silver is matched and used in the composite material layer, so that the silver is low in absorption loss and high in detection precision; the hexagonal carbon ring structure of the graphene oxide in the composite material layer has large specific surface area and good conductivity, the adsorption rate of analytes can be improved, three kinds of material interaction affect each other, compared with the arrangement of independent layers, metal particles Au-Ag can be adsorbed on oxygen-containing functional groups on the surface of GO through electrostatic action for nucleation and growth, GO can also be used as a protective layer, the phenomenon that metal particles are oxidized is avoided, and the synergistic enhancement effect of GO and metal particles is remarkable. Therefore, the Au-Ag-GO composite material layer of the sensor fully exerts the advantages of the three, and the sensitivity of the sensor is greatly improved. During measurement, the Au-Ag-GO composite material layer is sandwiched by the matching layer and the layer to be detected to form a long-range surface plasmon polariton propagation mode, the electromagnetic field of the long-range surface plasmon polariton propagation mode is symmetrically distributed about the central plane of the Au-Ag-GO composite material layer, the electromagnetic energy of the long-range surface plasmon polariton propagation mode is mainly concentrated in media on two sides of the Au-Ag-GO composite material layer, the limitation is small, the loss is low, the penetration depth of the long-range surface plasmon polariton propagation mode in the object to be detected can reach the micrometer or even centimeter magnitude, the surface electric field intensity of the long-range surface plasmon polariton propagation mode is enhanced, the penetration depth is increased, the application range of biosensing is greatly increased, and the detection capability is extended to the detection level of macromolecular cells.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic structural diagram of an Au-Ag-GO-based LRSPR high-sensitivity optical fiber sensor of the present invention;
FIG. 2 is a schematic structural diagram of an Au-Ag-GO-based LRSPR high-sensitivity optical fiber sensing unit of the utility model;
FIG. 3 is a graph obtained by linear fitting of the wavelength corresponding to the lowest point of the long-range resonance valley in the LRSPR effect and the corresponding refractive index value of the solution;
in the above figures: 1. the device comprises a wide-spectrum light source, 2, a glass tube, 3, an LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO, 4, a spectrometer, 5, a PC (personal computer), 6, a liquid inlet, 7, a liquid outlet, 8 and a support;
21. the method comprises the steps of a solution to be detected, 22, an optical fiber cladding, 23, an Au-Ag-GO composite material layer, 24, a matching layer, 25, transmitted light, 26 and an optical fiber core.
Detailed Description
In order to make the technical solutions and advantages of the present invention clearer, the following describes the technical solutions in the embodiments of the present invention clearly and completely with reference to the drawings in the embodiments of the present invention:
in the following examples, the PSS used has an average weight-average molecular weight Mw ≈ 70000, CAS: 25704-18-1.
In the following embodiments, a schematic structural diagram of an Au-Ag-GO based LRSPR high-sensitivity optical fiber sensing unit is shown in fig. 2, and includes an optical fiber core 26 with a removed optical fiber cladding 22, and a first optical fiber and a second optical fiber respectively connected to two ends of the optical fiber core with the removed optical fiber cladding, where the outer periphery of the optical fiber core with the removed optical fiber cladding is sequentially plated with a matching layer 24 and an Au-Ag-GO composite material layer 23 from inside to outside.
The diameter of the fiber core of the optical fiber is 200-300 μm, and the outer diameter of the optical fiber is 230-330 μm.
The matching layer is a fluorine-containing complex of terbium (III), and the thickness of the matching layer is 100-110 nm.
The thickness of the Au-Ag-GO composite material layer is 40-50 nm.
The matching layer is plated on the outer side of the optical fiber core without the optical fiber cladding by a dip coating method, and the Au-Ag-GO composite material layer is plated on the outer side of the matching layer film by a magnetron sputtering method.
The LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO can be matched with a wide-spectrum light source 1, a spectrometer 4 and a PC 5 for use to form an LRSPR high-sensitivity optical fiber sensor based on Au-Ag-GO, the structural schematic diagram of the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO is shown in figure 1, when detection is carried out, the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO is placed in a glass tube 2, a solution to be detected 21 is introduced into the glass tube 2 through a liquid inlet 6, the glass tube 2 is kept balanced through a bracket 8, the wide-spectrum light source 1 is arranged at the input end of the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO 3, transmission light 25 is transmitted into the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO 3, an LRSPR effect occurs during the transmission, the output end of the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO 3 is connected with the spectrometer 4, the spectrometer 4 is connected with the PC 5 through a data interface, and the wavelength corresponding to the lowest point of the long-range resonance valley under different solution refractive indexes detected by the spectrometer 4 is analyzed by the PC 5 to obtain a linear fitting result of the wavelength corresponding to the lowest point of the long-range resonance valley of the solution 21 to be detected and the corresponding solution refractive index value. After the detection is completed, the solution 21 to be detected is discharged through the liquid outlet 7.
Example 1
A first part: preparing optical fiber sensing unit
The preparation method of the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO comprises the following steps:
(1) preparation of matching layer Material
Research has shown that fluorine atom has low polarizability, high carbon-fluorine bond energy and short bond distance, so that the fluorine-containing material has low refractive index and good optical performance. Therefore, the matching layer material used in this experiment was selected among the fluorine-containing compounds. In consideration of the preparation cost and the current application situation, the experiment finally selects a terbium (III) fluorine-containing complex as a matching layer material, and the specific preparation method comprises the following steps: 1.15g of terbium acetate is taken to be put into a beaker, distilled water is added to the beaker to reach the scale of 20mL, and the mixture is stirred in an ice bath at the temperature of 0 ℃ until the mixture is completely dissolved; dripping 1.50mL of hexafluoroacetylacetone into the solution drop by drop, and stirring for 2-3 hours until white green precipitate is generated; and cleaning the precipitate with deionized water to obtain a product, and dissolving the white green crystal in absolute ethyl alcohol to finish the preparation of the matching layer solution.
(2) Preparation of Au-Ag-GO composite material
Firstly, 100mg of Graphene Oxide (GO) powder is weighed and added into 50-100mL of ultrapure water, and the graphene oxide suspension is formed by ultrasonic dispersion for 15 minutes.
In HAuCl at a concentration of 2-8mg/mL4In solution, the chitosan is mixed withHAuCl4Adding 10mg/mL chitosan solution at a mass ratio of 1:2, and uniformly stirring to obtain chitosan and HAuCl4The solution was mixed.
Adding chitosan and HAuCl4In a mixed solution according to HAuCl4With AgNO3In a molar ratio of 10:1, 2mg/mL of AgNO was added3And uniformly stirring the solution to obtain an Au-Ag mixed solution.
Mixing the above Au-Ag mixed solution with HAuCl4Mixing the suspension with the prepared graphene oxide suspension in a mass ratio of 1:1, and adding ascorbic acid in a mass ratio of 2:1 of ascorbic acid to graphene oxide. And finally, uniformly stirring the obtained solution, and centrifugally washing to obtain the Au-Ag-GO composite material.
(3) Matched layer plating
Selecting 2cm from the middle of an optical fiber, removing an optical fiber cladding, arranging a first optical fiber at one end without removing the optical fiber cladding and a second optical fiber at the other end, wherein the lengths of the first optical fiber and the second optical fiber are both 5cm, placing a clean optical fiber core without removing the optical fiber cladding in absolute ethyl alcohol for ultrasonic cleaning for 10 minutes to remove particulate matters on the surface of the optical fiber, then placing the optical fiber in acetone for ultrasonic cleaning for 15 minutes to remove organic impurities on the surface of the optical fiber, then taking out the optical fiber, repeatedly washing the optical fiber with a large amount of deionized water, and airing the optical fiber in clean air.
And then plating a matching layer on the surface of the cleaned optical fiber coating area by using a pulling coating instrument, wherein the coating speed is set to be 30 mm/min. The thickness of the matching layer is controlled to be 100-110nm by adjusting the concentration of the solution of the matching layer.
(4) Au-Ag-GO composite layer plating
And suspending the optical fiber plated with the matching layer into the vacuum cavity by using a fixing clamp, and adjusting the height of the fixing clamp to enable the fixing clamp to be 4cm away from the bottom of the vacuum cavity. Closing the vacuum chamber, and vacuumizing to 5 × 10-4Pa. At this time, hydrogen gas is filled with the flow rate of 13.3sccm, and a gate valve of the vacuum cavity is adjusted to stabilize the pressure of the hydrogen gas in the vacuum cavity at 0.6 Pa. The substrate rotation was turned on and the dc source voltage was adjusted to 297V and the current was adjusted to 0.04A. After pre-sputtering for 10 minutes, the target baffle is unscrewed for sputtering for a certain time.The thickness of the Au-Ag-GO composite material layer is controlled to be 40nm by controlling the sputtering time.
A second part: sensing experiment
The two sides of the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO are connected with a wide-spectrum light source 1 and a spectrometer 4, a solution to be detected flows through the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO through a liquid inlet and flows out of a liquid outlet 7, the spectrometer 4 is connected with a PC (personal computer) 5, and sensing phenomena are observed and recorded through the PC 5. The refractive indexes of the solutions to be detected in the experiment are respectively 1.330,1.334,1.338,1.342,1.346 and 1.350, the wavelengths corresponding to the lowest points of long-range resonance valleys when the LRSPR effect occurs are linearly fitted with the corresponding solution refractive index values, and a curve graph after fitting is shown in fig. 3, so that the sensitivity of the LRSPR high-sensitivity optical fiber sensor based on Au-Ag-GO is 11290nm/RIU and is far higher than that of the optical fiber sensor of the same type.
Example 2
An LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO comprises an optical fiber core with an optical fiber cladding removed, wherein one end of the optical fiber core with the optical fiber cladding removed is connected with a first optical fiber, the other end of the optical fiber core with the optical fiber cladding removed is connected with a second optical fiber, the periphery of the optical fiber core with the optical fiber cladding removed is sequentially plated with a matching layer and an Au-Ag-GO composite material layer from inside to outside, and the matching layer is made of a terbium (III) fluorine-containing complex.
The diameter of the fiber core of the optical fiber is 200 μm, and the thickness of the cladding is 30 μm.
The thickness of the matching layer is 100 nm.
The thickness of the Au-Ag-GO composite material layer is 40 nm.
The matching layer is plated on the outer side of the optical fiber core without the optical fiber cladding by a dip coating method, and the Au-Ag-GO composite material layer is plated on the outer side of the matching layer by a magnetron sputtering method.
Comparative example 1
An LRSPR fiber sensor as in example 1, except that Au-Ag-GO is not a composite material, but first Au layer, then Ag layer, and finally GO layer, has the following sensitivity: 3456nm/RIU, which shows that after recombination, the sensitivity is greatly enhanced.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and equivalent alternatives or modifications according to the technical solution of the present invention and the inventive concept thereof should be covered by the scope of the present invention.
Claims (9)
1. The LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO is characterized by comprising an optical fiber core with an optical fiber cladding removed, wherein one end of the optical fiber core with the optical fiber cladding removed is connected with a first optical fiber, the other end of the optical fiber core with the optical fiber cladding removed is connected with a second optical fiber, and a matching layer and an Au-Ag-GO composite material layer are sequentially arranged on the periphery of the optical fiber core with the optical fiber cladding removed from the inner side to the outer side.
2. The Au-Ag-GO based LRSPR high-sensitivity optical fiber sensing unit according to claim 1, wherein the diameter of the optical fiber core without the optical fiber cladding is 200-300 μm, the diameters of the core of the first optical fiber and the second optical fiber are the same as the diameter of the optical fiber core without the optical fiber cladding, and the optical fiber cores are coaxial; the fiber cladding of the first optical fiber is equal to that of the second optical fiber, and the thickness of the fiber cladding of the first optical fiber is 20-30 mu m.
3. The Au-Ag-GO based LRSPR high sensitivity fiber sensing unit according to claim 1, wherein the length of the fiber core from which the cladding is removed is 2cm, the length of the first fiber is 5cm and the length of the second fiber is 5 cm.
4. The Au-Ag-GO-based LRSPR high-sensitivity optical fiber sensing unit according to claim 1, wherein the matching layer is terbium (III) fluorine-containing complex, and the thickness of the matching layer is 100-110 nm.
5. The Au-Ag-GO-based LRSPR high-sensitivity optical fiber sensing unit according to claim 1, wherein the thickness of the Au-Ag-GO composite material layer is 40-50 nm.
6. An LRSPR high-sensitivity optical fiber sensor based on Au-Ag-GO, which is characterized by comprising the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO of any one of claims 1 to 5, and further comprising a light source, a spectrometer and a PC; the light source is arranged at the input end of the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO, the output end of the LRSPR high-sensitivity optical fiber sensing unit based on Au-Ag-GO is connected with the spectrometer, and the spectrometer is connected with the PC.
7. The Au-Ag-GO based LRSPR high sensitivity optical fiber sensor of claim 6, wherein the wavelength range of the spectrum is 500-800 nm.
8. The Au-Ag-GO based LRSPR high sensitivity optical fiber sensor of claim 6, wherein the wavelength range of the spectrometer is 200-1100 nm.
9. The Au-Ag-GO based LRSPR high sensitivity optical fiber sensor according to claim 6, wherein the detection sensitivity of the Au-Ag-GO based LRSPR high sensitivity optical fiber sensor is as follows: 9600-12000 nm/RIU.
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