CN111650158A - Cu2+Concentration detection device and preparation method thereof - Google Patents
Cu2+Concentration detection device and preparation method thereof Download PDFInfo
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- 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
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
- G01N21/45—Refractivity; Phase-affecting properties, e.g. optical path length using interferometric methods; using Schlieren methods
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- G01D5/00—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable
- G01D5/26—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light
- G01D5/32—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light with attenuation or whole or partial obturation of beams of light
- G01D5/34—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light with attenuation or whole or partial obturation of beams of light the beams of light being detected by photocells
- G01D5/353—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light with attenuation or whole or partial obturation of beams of light the beams of light being detected by photocells influencing the transmission properties of an optical fibre
- G01D5/35306—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light with attenuation or whole or partial obturation of beams of light the beams of light being detected by photocells influencing the transmission properties of an optical fibre using an interferometer arrangement
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- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
- G01N21/45—Refractivity; Phase-affecting properties, e.g. optical path length using interferometric methods; using Schlieren methods
- G01N2021/458—Refractivity; Phase-affecting properties, e.g. optical path length using interferometric methods; using Schlieren methods using interferential sensor, e.g. sensor fibre, possibly on optical waveguide
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Abstract
The invention discloses a Cu2+Concentration detection device and preparation method thereof, wherein, the device include optical fiber sensor, through optic fibre with the broadband light source that optical fiber sensor one end is connected to and through optic fibre with the fiber optic spectrometer that the optical fiber sensor other end is connected, optical fiber sensor includes bipyramid optical fiber structure and cladding the polymer rete on bipyramid optical fiber structure surface, the polymer rete is the n rete that modified carbon nanotube layer and polyacrylic acid layer formed in turn, bipyramid optical fiber structure comprises two micro-nano optical fiber cascades, micro-nano optical fiber is formed by single mode fiber tapering preparation. By using Cu of the present invention2+Concentration detection device for Cu2+The method for detecting the concentration is simple and convenient to operate, low in cost, easy to carry and high in sensitivity.
Description
Technical Field
The invention relates to the field of heavy metal ion concentration sensors, in particular to Cu2+A concentration detection device and a preparation method thereof.
Background
Over the years, with the development of industry and technology, the pollution of soil, rivers and even drinking water has become increasingly serious. Wastewater from mining, corrosion and electronics manufacturing industries contains large amounts of harmful heavy metal ions and other impurities. Heavy metals are a group of metals with high atomic weight and relatively high density, and are toxic even at low concentrations. The increase in industrial activity has led to the entry of heavy metals into the environment through air, water and soil. Copper is the third most abundant heavy metal content essential to human body, and plays an important role in various physiological processes. Copper also has multiple functions, such as iron absorption, hematopoiesis, multiple enzyme activities, and redox processes. However, excessive copper intake may lead to diarrhea, vomiting, kidney or liver disease. Cu commonly used2+The detection method comprises a colorimetric method, a fluorescence method, an anodic stripping voltammetry method and an atomic absorption method. While these methods generally provide highly sensitive, highly selective, or multi-element assays, they are time consuming, complex, expensive, and require sample preparation and special operational training.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the above-mentioned deficiencies of the prior art, it is an object of the present invention to provide a Cu2+A concentration detection device and a preparation method thereof, aiming at solving the problem of the existing Cu2+The detection method has the problems of complex operation, time consumption and high cost.
The technical scheme of the invention is as follows:
cu2+Concentration detection device, wherein, including optical fiber sensor, through optic fibre with the broadband light source that optical fiber sensor one end is connected to and through optic fibre with the optical fiber spectrometer that the optical fiber sensor other end is connected, optical fiber sensor includes bipyramid optical fiber structure and cladding in the polymer rete on bipyramid optical fiber structure surface, the polymer rete is the n rete that modified carbon nanotube layer and polyacrylic acid layer formed in turn, bipyramid optical fiber structure comprises two micro-nano optical fiber cascades,the micro-nano optical fiber is prepared by tapering a single-mode optical fiber.
The Cu2+The concentration detection device is provided, wherein n is more than or equal to 10 and less than or equal to 30.
The Cu2+The concentration detection device further comprises a fixing clamp used for fixing the optical fiber.
The Cu2+And the concentration detection device is characterized in that a glass slide is arranged below the optical fiber sensor.
The Cu2+The concentration detection device comprises a broadband light source, wherein the light source wavelength range of the broadband light source is 1200-1700 nm.
The Cu2+The preparation method of the concentration detection device comprises the following steps:
providing a broadband light source and a fiber optic spectrometer;
melting and tapering a single-mode optical fiber by using an optical fiber fusion splicer to obtain a first micro-nano optical fiber, preparing a second micro-nano optical fiber with the same parameters behind the first micro-nano optical fiber, and cascading the first micro-nano optical fiber and the second micro-nano optical fiber together to form a biconical optical fiber structure;
preparing n-layer films formed by sequentially and alternately forming a modified carbon nanotube layer and a polyacrylic acid layer on the surface of the biconical optical fiber structure to prepare an optical fiber sensor;
connecting the two ends of the optical fiber sensor with the broadband light source and the optical fiber spectrometer respectively through optical fibers to obtain the Cu2+A concentration detection device.
The Cu2+The preparation method of the concentration detection device comprises the following steps of preparing n-layer films formed by sequentially and alternately forming a modified carbon nanotube layer and a polyacrylic acid layer on the surface of the biconical optical fiber structure, and preparing the optical fiber sensor, wherein the steps of preparing the optical fiber sensor comprise:
putting the biconical optical fiber structure into a mixed solution of concentrated sulfuric acid and hydrogen peroxide, and heating to obtain a pretreated biconical optical fiber structure;
putting the pretreated biconical optical fiber structure into a modified carbon nanotube solution, and forming a modified carbon nanotube layer on the surface of the pretreated biconical optical fiber structure;
putting the pretreated biconical optical fiber structure with the modified carbon nanotube layer formed on the surface into a polyacrylic acid solution, and generating a polyacrylic acid layer on the surface of the modified carbon nanotube layer;
repeating the film coating process to obtain n-layer films formed by sequentially and alternately arranging a modified carbon nanotube layer and a polyacrylic acid layer on the surface of the pretreated biconical optical fiber structure;
and drying the pretreated biconical optical fiber structure after the film coating is finished, so that the modified carbon nanotube layer and the polyacrylic acid layer are fully reacted and combined to obtain the optical fiber sensor.
The Cu2+The preparation method of the concentration detection device comprises the step of drying the pretreated biconical optical fiber structure after coating at the temperature of 50-80 ℃ for 3-5 hours.
The Cu2+The preparation method of the concentration detection device comprises the following steps of:
adding carbon nano tubes into a concentrated nitric acid solution, treating for 6 hours at 120 ℃, cooling, carrying out suction filtration, washing with distilled water for three times, placing in a vacuum drying oven for drying for 8 hours, and grinding to obtain modified carbon nano tubes;
adding the modified carbon nano tube into an acetic acid solution with the concentration of 4%, carrying out ultrasonic treatment, and then carrying out magnetic stirring for 2h at the temperature of 80 ℃ to obtain a modified carbon nano tube solution.
The Cu2+The preparation method of the concentration detection device is characterized in that the concentration of the modified carbon nanotube solution is 1 wt%, and the concentration of the polyacrylic acid solution is 35 wt%.
Has the advantages that: the invention provides a Cu2+Concentration detection device, it includes the bipyramid fiber structure that two micro-nano optical fiber cascade constitute, bipyramid fiber structure surface cladding has the polymer rete of being in turn formed by modified carbon nanotube layer and polyacrylic acid layer in proper order, the surface cladding has the bipyramid fiber structure constitution optical fiber sensor of polymer rete. Dropwise adding a solution to be detected to the surface of the optical fiber sensor, wherein the solution to be detectedCu of (2)2+The volume change of the polymer film layer on the surface of the optical fiber sensor can be caused, the refractive index is changed, the intensity change of the interference spectrum transmission peak of the optical fiber sensor is caused, and the Cu in the solution to be detected is obtained according to the intensity change of the interference spectrum transmission peak2+And (4) concentration. By using Cu of the present invention2+Concentration detection device for Cu2+The method for detecting the concentration is simple and convenient to operate, low in cost, easy to carry and high in sensitivity.
Drawings
FIG. 1 shows a Cu alloy of the present invention2+The structure of the preferred embodiment of the concentration detection device is shown schematically.
Fig. 2 is a schematic structural diagram of the optical fiber sensor of the present invention.
FIG. 3 shows a Cu alloy of the present invention2+A flow chart of a preferred embodiment of a method for making a concentration detection device.
Detailed Description
The invention provides a Cu2+The concentration detection device and the preparation method thereof are further described in detail below in order to make the objects, technical solutions, and effects of the present invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The optical fiber sensor has the advantages of small volume, low cost, electromagnetic interference resistance, multiplexing resistance and the like. Among various types of optical fiber sensors, the interferometric sensor has attracted much attention because of its advantages of large dynamic range, high sensitivity, high precision, etc. The most commonly used fiber optic interferometers are the michelson type, the sagnac type, the fabry-perot type and the mach-zehnder type. Of these interferometers, the mach-zehnder interferometer (MZ) configuration has significant advantages such as simplicity of manufacture, direct reading, and relatively high sensitivity.
The embodiment of the invention provides Cu based on a Mach-Zehnder interferometer2+A concentration detecting apparatus, as shown in FIGS. 1 and 2, includes an optical fiber sensor 10, a broadband light source 20 connected to one end of the optical fiber sensor 10 through an optical fiber, and another optical fiber sensor 10 connected to the other end of the optical fiber sensor through an optical fiberEnd connection's fiber optic spectrometer 30, optical fiber sensor 10 includes bipyramid optical fiber structure 11 and cladding in the polymer rete 12 on bipyramid optical fiber structure 11 surfaces, polymer rete 12 is the n rete that modified carbon nanotube layer and polyacrylic acid layer formed in turn in proper order, bipyramid optical fiber structure 11 comprises two micro-nano optical fiber cascades, micro-nano optical fiber is formed by single mode fiber tapering preparation.
In this embodiment, the broadband light source emits a light source, the light source is transmitted to the optical fiber sensor through an optical fiber, and when the solution to be measured is dripped to the surface of the optical fiber sensor, Cu in the solution to be measured2+The volume change of the polymer film layer on the surface of the optical fiber sensor is caused, the refractive index is changed, and the intensity change of the transmission peak of the interference spectrum of the optical fiber sensor is caused, and the optical fiber spectrometer 30 can obtain the Cu in the solution to be measured according to the intensity change of the transmission peak of the interference spectrum2+And (4) concentration. Using Cu of this example2+Concentration detection device for Cu2+The method for detecting the concentration is simple and convenient to operate, low in cost, easy to carry and high in sensitivity.
Because the amino functional group in the polymer film layer formed by the modified carbon nano tube and the polyacrylic acid layer can provide lone pair electrons, the amino functional group can be used as a metal ion chelating agent to react with Cu in a solution to be detected2+Generates complexation, forms stable complex through coordination bond, has larger specific surface area and abundant void structure on the surface of the modified carbon nano tube, and can adsorb Cu through electrostatic interaction2+And (3) solution. Therefore, when the optical fiber sensor plated with the polymer film is used for testing a solution to be tested, the chelating effect can cause the refractive index of the polymer film to change, and further cause the change of an interference spectrum, and the optical fiber spectrometer 30 can obtain Cu in the solution to be tested according to the change of the transmission peak intensity of the interference spectrum2+And (4) concentration.
In some embodiments, the broadband light source is a special device in the field of optical fiber sensing and optical fiber communication, has the advantages of wide wavelength range, high output power and the like, and can provide input light for the M-Z interference optical fiber sensor. By way of example, the broadband light source emits light in the wavelength range of 1200-1700 nm.
In some embodiments, as shown in fig. 2, the optical fiber sensor 10 includes a biconical optical fiber structure 11 and a polymer film layer 12 coated on a surface of the biconical optical fiber structure 11, where the biconical optical fiber structure 11 is formed by cascading two micro-nano optical fibers, and the micro-nano optical fibers are prepared by tapering a single-mode optical fiber. In this embodiment, when light emitted from the broadband light source reaches the first micro-nano fiber, a part of fundamental modes in the core of the single-mode fiber are excited into the fiber cladding and become fiber cladding modes. Meanwhile, the rest part of the fiber core fundamental mode continues to remain in the fiber core for transmission. The middle part of the two micro-nano optical fibers is used as a sensing interference arm. When the light transmitted in the fiber cladding reaches the second micro-nano fiber, the cladding mode in the fiber cladding is coupled back into the fiber core and interferes with the fundamental mode transmitted in the fiber core. And because a phase difference exists between the fundamental mode in the fiber core and the high-order mode in the cladding, an interference peak is generated, and the Mach-Zehnder interferometer is formed. The interfered light is continuously transmitted in the fiber core of the optical fiber, and finally is regulated and displayed through the optical fiber spectrometer.
In some embodiments, as shown in FIG. 1, the Cu2+The concentration detection device further comprises a fixing clamp 40 for fixing the optical fiber, and a glass slide for bearing the solution to be detected is arranged below the optical fiber sensor 10.
In some embodiments, the polymer film layer 12 is a 10-30 layer film formed by alternating a modified carbon nanotube layer and a polyacrylic acid layer. In some specific embodiments, in order to explore the optimal number of coating layers, polymer film layers with different coating layers are respectively coated on the surface of the biconical optical fiber structure, and the Mach-Zehnder optical fiber sensor functionalized by the polymer film layers is placed in Cu with different concentrations2+Experimental measurements were performed in solution. The results of comparative experiments show that the optimal number of the film layers is 16, and the sensitivity of the sensor can reach 18.4598dB/mM when the concentration of copper ions is 0.1-1.0 mM.
In some embodiments, there is also provided Cu2+The method for manufacturing the concentration detecting device, as shown in FIG. 3, includes the steps of：
S10, providing a broadband light source and a fiber optic spectrometer;
s20, melting and tapering the single-mode optical fiber by using an optical fiber fusion splicer to obtain a first micro-nano optical fiber, preparing a second micro-nano optical fiber with the same parameters behind the first micro-nano optical fiber, and cascading the first micro-nano optical fiber and the second micro-nano optical fiber together to form a double-cone optical fiber structure;
s30, preparing n-layer films formed by sequentially and alternately forming a modified carbon nanotube layer and a polyacrylic acid layer on the surface of the biconical optical fiber structure to obtain the optical fiber sensor;
s40, respectively connecting the two ends of the optical fiber sensor with the broadband light source and the optical fiber spectrometer through optical fibers to obtain the Cu2+A concentration detection device.
In some embodiments, the fabrication of the biconic fiber structure comprises the steps of: the micro-nano optical fiber is prepared by melting and tapering a single mode optical fiber by utilizing a polarization maintaining optical fiber fusion splicer (FSM-100P +, Fujikura). Firstly, removing a coating layer of a common single-mode optical fiber by using an optical fiber wire stripper, wiping the surface of the optical fiber by using alcohol, then cutting the end surface of the single-mode optical fiber to be flat by using an optical fiber cutter, and finally putting the single-mode optical fiber into a polarization-maintaining optical fiber fusion splicer for fusion splicing and tapering. In the preparation process of the micro-nano optical fiber, firstly, the single-mode optical fiber is heated to a molten state through the discharge of two electrode rods of the polarization-maintaining fusion splicer, and meanwhile, a stepping motor of the polarization-maintaining fusion splicer moves in an accelerated manner, so that the optical fiber is thinned to the diameter to be prepared. In the process, the micro-nano optical fiber conical transition regions with different gradient degrees can be obtained by adjusting the initial speed and the acceleration of the stepping motor. After the acceleration of the stepping motor is set, the micro-nano optical fibers with different diameters can be obtained by controlling the movement time of the stepping motor. And then, the step motor is controlled to stretch the optical fiber at a constant speed, so that the micro-nano optical fibers with different lengths are obtained. Meanwhile, the movement time of the stepping motor is kept consistent with the discharge time of the electrode rod, so that the single-mode optical fiber is always in a heating and melting state in the movement process of the stepping motor. According to the same method, a micro-nano optical fiber with the same parameters is prepared behind the prepared micro-nano optical fiber, so that the Mach-Zehnder interferometer (namely a biconical optical fiber structure) is formed by utilizing the two micro-nano optical fibers which are cascaded together.
In some embodiments, the polymer film layer is formed by sequential alternating self-assembly of a modified carbon nanotube layer and a polyacrylic acid layer through electrostatic interaction, and the optical fiber sensor comprises:
s31, putting the biconical optical fiber structure into a mixed solution of concentrated sulfuric acid and hydrogen peroxide, and heating to obtain a pretreated biconical optical fiber structure;
s32, putting the pretreated biconical optical fiber structure into a modified carbon nanotube solution, and forming a modified carbon nanotube layer on the surface of the pretreated biconical optical fiber structure;
s33, putting the pretreated biconical optical fiber structure with the modified carbon nanotube layer formed on the surface into a polyacrylic acid solution, and generating a polyacrylic acid layer on the surface of the modified carbon nanotube layer;
s34, repeating the film coating process, and obtaining n-layer films formed by the modified carbon nanotube layer and the polyacrylic acid layer alternately in sequence on the surface of the pretreated biconical optical fiber structure;
and S35, drying the pretreated biconical optical fiber structure after film coating, so that the modified carbon nanotube layer and the polyacrylic acid layer are fully reacted and combined to obtain the optical fiber sensor.
The optical fiber sensor manufactured by the embodiment has the advantages of simplicity in preparation, easiness in signal light transmission, high stability, strong anti-electromagnetic interference capability, corrosion resistance, high sensitivity and the like, and also has the advantages of low cost, light weight, small size, simple structure, high mechanical strength and the like, so that the measuring equipment and cost are reduced, and the optical fiber sensor can be widely applied to the fields of water quality detection, environment monitoring and the like.
Specifically, the embodiment pre-disposes a modified carbon nanotube solution and a polyacrylic acid solution, wherein the preparation of the modified carbon nanotube solution comprises the steps of: adding carbon nano tubes into a certain amount of concentrated nitric acid solution, treating for 6 hours at 120 ℃, cooling, carrying out suction filtration, washing for three times by using distilled water, placing in a vacuum drying oven for drying for 8 hours, and grinding to obtain modified carbon nano tubes; adding 50g of modified carbon nano tube into 50ml of 4% acetic acid solution, carrying out ultrasonic treatment for 3min, and then carrying out magnetic stirring at 80 ℃ for 2h to obtain 1 wt% modified carbon nano tube solution; the surface of the modified carbon nano tube contains functional groups such as hydroxyl, amino, carbonyl and the like, and the amino can be protonated and positively charged in an acidic solution; the preparation of the polyacrylic acid solution comprises the following steps: by diluting polyacrylic acid with deionized water to obtain a 35 wt% polyacrylic acid solution, deprotonation of the carboxyl groups in the polyacrylic acid solution occurs with negative charge.
Secondly, the manufactured biconical optical fiber structure is put into piranha solution (98% concentrated sulfuric acid and 30% hydrogen peroxide) for treatment, the mixture is heated for 1 hour at the temperature of 80 ℃, organic matter residues on the surface of the optical fiber structure are removed, the surface of the optical fiber structure is hydroxylated, then the optical fiber structure is fully cleaned for a plurality of times by deionized water and ethanol, and the optical fiber structure is dried in a drying box, so that the pretreated biconical optical fiber structure is obtained.
Secondly, putting the pretreated optical fiber sensor into the 1 wt% modified carbon nanotube solution for full reaction for 2min, then slowly taking out, drying in the air for 1min, and forming a modified carbon nanotube layer on the surface of the pretreated biconical optical fiber structure; then, putting the carbon nano tube into 35 wt% polyacrylic acid solution, slowly taking out after 2min, and drying in the air for 1min to generate a polyacrylic acid layer on the surface of the modified carbon nano tube layer; finally, the membrane was again placed in deionized water for 2 minutes to remove loosely bound molecules, and then slowly removed and dried in air for 1 minute. Because the modified carbon nanotube layer is positively charged and the polyacrylic acid layer is negatively charged, the modified carbon nanotube layer and the polyacrylic acid layer can be assembled layer by layer through electrostatic adsorption to form a uniform polymer film layer. The complete multilayer polymer film layer can be obtained by repeating the film coating process, and the optical fiber sensor after film coating is placed in a constant temperature drying oven to be heated for 3-5h at the temperature of 50-80 ℃ so that the modified carbon nano tube and polyacrylic acid are fully reacted and combined.
In the invention, because the amino functional group in the polymer film layer formed by the modified carbon nano tube and the polyacrylic acid layer can provide lone pair electrons, the amino functional group can be used as a metal ion chelating agent to be mixed with Cu in a solution to be detected2+Generates complexation, forms stable complex through coordination bond, has larger specific surface area and abundant void structure on the surface of the modified carbon nano tube, and can adsorb Cu through electrostatic interaction2+And (3) solution. Therefore, when the optical fiber sensor plated with the polymer film is used for testing a solution to be tested, the chelating effect can cause the refractive index of the polymer film to change, and further cause the change of an interference spectrum, and the optical fiber spectrometer 30 can obtain Cu in the solution to be tested according to the change of the transmission peak intensity of the interference spectrum2+And (4) concentration.
In summary, the present invention provides a Cu2+Concentration detection device, it includes the bipyramid fiber structure that two micro-nano optical fiber cascade constitute, bipyramid fiber structure surface cladding has the polymer rete of being in turn formed by modified carbon nanotube layer and polyacrylic acid layer in proper order, the surface cladding has the bipyramid fiber structure constitution optical fiber sensor of polymer rete. Dropwise adding a solution to be detected to the surface of the optical fiber sensor, wherein Cu in the solution to be detected2+The volume change of the polymer film layer on the surface of the optical fiber sensor can be caused, the refractive index is changed, the intensity change of the interference spectrum transmission peak of the optical fiber sensor is caused, and the Cu in the solution to be detected is obtained according to the intensity change of the interference spectrum transmission peak2+And (4) concentration. By using Cu of the present invention2+Concentration detection device for Cu2+The method for detecting the concentration is simple and convenient to operate, low in cost, easy to carry and high in sensitivity.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. Cu2+The concentration detection device is characterized by comprising an optical fiber sensor, a broadband light source connected with one end of the optical fiber sensor through an optical fiber, and an optical fiber spectrometer connected with the other end of the optical fiber sensor through the optical fiber, wherein the optical fiber sensor comprises a biconical optical fiber structure and a packageThe polymer film layer covers the surface of the biconical optical fiber structure, the polymer film layer is an n-layer film formed by a modified carbon nano tube layer and a polyacrylic acid layer in turn, the biconical optical fiber structure is formed by cascading two micro-nano optical fibers, and the micro-nano optical fibers are formed by tapering single-mode optical fibers.
2. Cu according to claim 12+The concentration detection device is characterized in that n is more than or equal to 10 and less than or equal to 30.
3. Cu according to claim 12+The concentration detection device is characterized by further comprising a fixing clamp used for fixing the optical fiber.
4. Cu according to claim 12+The concentration detection device is characterized in that a glass slide is arranged below the optical fiber sensor.
5. Cu according to claim 12+The concentration detection device is characterized in that the light source wavelength range of the broadband light source is 1200-1700 nm.
6. Cu as claimed in any of claims 1 to 52+The preparation method of the concentration detection device is characterized by comprising the following steps:
providing a broadband light source and a fiber optic spectrometer;
melting and tapering a single-mode optical fiber by using an optical fiber fusion splicer to obtain a first micro-nano optical fiber, preparing a second micro-nano optical fiber with the same parameters behind the first micro-nano optical fiber, and cascading the first micro-nano optical fiber and the second micro-nano optical fiber together to form a biconical optical fiber structure;
preparing n-layer films formed by sequentially and alternately forming a modified carbon nanotube layer and a polyacrylic acid layer on the surface of the biconical optical fiber structure to prepare an optical fiber sensor;
connecting the two ends of the optical fiber sensor with the broadband light source and the optical fiber spectrometer respectively through optical fibers to obtain the Cu2+A concentration detection device.
7. Cu according to claim 62+The preparation method of the concentration detection device is characterized in that n-layer films formed by sequentially and alternately forming a modified carbon nanotube layer and a polyacrylic acid layer are prepared on the surface of the biconical optical fiber structure, and the step of preparing the optical fiber sensor comprises the following steps:
putting the biconical optical fiber structure into a mixed solution of concentrated sulfuric acid and hydrogen peroxide, and heating to obtain a pretreated biconical optical fiber structure;
putting the pretreated biconical optical fiber structure into a modified carbon nanotube solution, and forming a modified carbon nanotube layer on the surface of the pretreated biconical optical fiber structure;
putting the pretreated biconical optical fiber structure with the modified carbon nanotube layer formed on the surface into a polyacrylic acid solution, and generating a polyacrylic acid layer on the surface of the modified carbon nanotube layer;
repeating the film coating process to obtain n-layer films formed by sequentially and alternately arranging a modified carbon nanotube layer and a polyacrylic acid layer on the surface of the pretreated biconical optical fiber structure;
and drying the pretreated biconical optical fiber structure after the film coating is finished, so that the modified carbon nanotube layer and the polyacrylic acid layer are fully reacted and combined to obtain the optical fiber sensor.
8. Cu according to claim 72+The preparation method of the concentration detection device is characterized in that the temperature for drying the pretreated biconical optical fiber structure after coating is 50-80 ℃ for 3-5 hours.
9. Cu according to claim 72+The preparation method of the concentration detection device is characterized in that the preparation of the modified carbon nanotube solution comprises the following steps:
adding carbon nano tubes into a concentrated nitric acid solution, treating for 6 hours at 120 ℃, cooling, carrying out suction filtration, washing with distilled water for three times, placing in a vacuum drying oven for drying for 8 hours, and grinding to obtain modified carbon nano tubes;
adding the modified carbon nano tube into an acetic acid solution with the concentration of 4%, carrying out ultrasonic treatment, and then carrying out magnetic stirring for 2h at the temperature of 80 ℃ to obtain a modified carbon nano tube solution.
10. Cu according to claim 72+The preparation method of the concentration detection device is characterized in that,
the concentration of the modified carbon nanotube solution is 1 wt%, and the concentration of the polyacrylic acid solution is 35 wt%.
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Application publication date: 20200911 |