CN110736722B - Manufacturing method of graphene quantum dot composite material optical fiber gas sensor - Google Patents
Manufacturing method of graphene quantum dot composite material optical fiber gas sensor Download PDFInfo
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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
- G01N21/41—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
- B82—NANOTECHNOLOGY
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/02—Optical fibres with cladding with or without a coating
- G02B6/02057—Optical fibres with cladding with or without a coating comprising gratings
- G02B6/02076—Refractive index modulation gratings, e.g. Bragg gratings
- G02B6/0208—Refractive index modulation gratings, e.g. Bragg gratings characterised by their structure, wavelength response
- G02B6/021—Refractive index modulation gratings, e.g. Bragg gratings characterised by their structure, wavelength response characterised by the core or cladding or coating, e.g. materials, radial refractive index profiles, cladding shape
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/02—Optical fibres with cladding with or without a coating
- G02B6/02295—Microstructured optical fibre
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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
- G01N21/41—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
Abstract
The invention discloses a preparation method of an optical fiber gas sensor, wherein the optical fiber sensor consists of a first single-mode optical fiber, a first multimode optical fiber, a photonic crystal optical fiber, a second multimode optical fiber and a second single-mode optical fiber, wherein two ends of the photonic crystal optical fiber are respectively connected with the first multimode optical fiber and the second multimode optical fiber, two ends of the first multimode optical fiber and the second multimode optical fiber are respectively welded with the first single-mode optical fiber and the second single-mode optical fiber, and the surface of the photonic crystal optical fiber is coated with a titanium dioxide/aminated graphene quantum dot composite sensitive film; the preparation method comprises the steps of preparing the titanium dioxide/aminated graphene quantum dot composite material, coating the titanium dioxide/aminated graphene quantum dot composite material on the photonic crystal fiber to form a detection film, and welding a plurality of sections of optical fibers to form the interferometer. The graphene quantum dot composite material optical fiber gas sensor is low in manufacturing cost, small in size, simple and stable in structure and easy to prepare.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a method for manufacturing a graphene quantum dot composite material optical fiber gas sensor.
Background
Hydrogen sulfide (H)2S) is colorless, extremely toxic and acidic gas, and even in the case of low concentration, human smell is damaged, so that low concentration H is prevented2The monitoring of S is very important. In the sensitive material, the functionalized graphene quantum dot is a two-dimensional carbon material in which graphene contains heterogeneous atoms/molecules and the aminated graphene quantum dot-nitrogen-containing group is surface-modified to form a bond. The aminated graphene quantum dot has a large specific surface area and rich oxygen-containing functional groups, so that the titanium dioxide/aminated graphene quantum dot and H2The contact area of S gas is large, so that H is adsorbed2S gas is easier. The traditional hydrogen sulfide sensor has long detection response time and high manufacturing cost.
The optical fiber sensing technology is a new high technology with a wide prospect in development. The optical fiber has a plurality of special properties in the process of transmitting information, for example, the energy loss is very small when the optical fiber transmits information, thereby bringing great convenience to remote measurement. The optical fiber material has stable performance, is not interfered by an electromagnetic field, and is kept unchanged under severe environments such as high temperature, high pressure, low temperature, strong corrosion and the like, so that the optical fiber sensor is developed rapidly from the appearance to the present. Therefore, how to use the optical fiber sensing technology to manufacture a gas sensor for detecting the concentration of low-concentration hydrogen sulfide, so that the gas sensor has the effects of stable operation, good detection effect, fast response time, high precision and reliability and the like, becomes a problem to be further considered.
Disclosure of Invention
The invention aims to provide a method for manufacturing a graphene quantum dot composite material optical fiber gas sensor, and aims to detect low-concentration hydrogen sulfide through the optical fiber gas sensor and improve detection precision and reliability.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a novel optical fiber gas sensor comprises the following steps that the optical fiber sensor is composed of a first single mode optical fiber, a first multimode optical fiber, a photonic crystal optical fiber, a second multimode optical fiber and a second single mode optical fiber, two ends of the photonic crystal optical fiber are respectively connected with the first multimode optical fiber and the second multimode optical fiber, two ends of the first multimode optical fiber and two ends of the second multimode optical fiber are respectively welded with the first single mode optical fiber and the second single mode optical fiber, and the surface of the photonic crystal optical fiber is coated with a titanium dioxide/aminated graphene quantum dot composite sensitive film; the method specifically comprises the following steps:
step 1: preparing a titanium dioxide/aminated graphene quantum dot composite material solution;
step 2: and coating the prepared titanium dioxide/aminated graphene quantum dot composite material on a photonic crystal fiber to form a detection film.
And step 3: the two ends of the coated photonic crystal fiber are cut flat by using a fiber cutter, the length of the photonic crystal fiber is kept at 4.5cm, the two ends of the cut section are respectively welded with a section of multimode fiber in a tapering welding mode by using a fiber welding machine, and then the two sections of multimode fiber are respectively welded with a section of single-mode fiber.
Compared with the prior art, the invention has the following beneficial effects: according to the invention, the photonic crystal fiber is coated with the titanium dioxide/aminated graphene quantum dot composite sensitive film, the titanium dioxide can effectively improve the sensitivity of the optical fiber sensor to hydrogen sulfide gas, the precision and reliability of the single graphene used as the gas sensor are improved, and the movement of an interference wave peak is detected by the spectrum detector, so that the hydrogen sulfide gas can be detected; the graphene quantum dot composite material optical fiber gas sensor is low in manufacturing cost, small in size, simple and stable in structure and easy to prepare.
Drawings
Fig. 1 is a schematic diagram of a method for manufacturing an optical fiber gas sensor according to an embodiment of the present invention.
FIG. 2 is a schematic diagram of linear fitting of wavelength shift and wavelength for detecting hydrogen sulfide gas with different concentrations according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of an optical fiber gas sensor, wherein the optical fiber sensor consists of a first single-mode optical fiber, a first multimode optical fiber, a photonic crystal optical fiber, a second multimode optical fiber and a second single-mode optical fiber, wherein two ends of the photonic crystal optical fiber are respectively connected with the first multimode optical fiber and the second multimode optical fiber, and two ends of the first multimode optical fiber and the second multimode optical fiber are respectively welded with the first single-mode optical fiber and the second single-mode optical fiber; wherein, the optical surface of the photonic crystal is coated with a layer of titanium dioxide/aminated graphene quantum dot composite sensitive film; the method specifically comprises the preparation of a sensing element and the preparation of a titanium dioxide/aminated graphene quantum dot composite material, and comprises the following steps:
step 1: preparing a titanium dioxide/aminated graphene quantum dot composite material solution; the configuration process specifically comprises the following steps: weighing 0.04g of nano titanium dioxide with the particle size of 5-10nm by using an electronic balance, dispersing the nano titanium dioxide in 50ml of deionized water, preparing a nano titanium dioxide aqueous solution, adding a stirrer, and covering a preservative film; stirring the mixed solution on a constant-temperature heating magnetic stirrer, taking 1ml of the mixed solution in a small test tube by using a pipette, taking 1ml of aminated graphene quantum dots with the concentration of 1mg/ml and the particle size of 2.5-4.5nm, mixing the aminated graphene quantum dots with the aminated graphene quantum dots, and putting the mixture in a mechanical ultrasonic cleaning machine for treatment; in the ultrasonic process, the temperature is controlled to be lower than 4 ℃, ultrasonic treatment is carried out for 20 minutes, the process is strictly sealed and is stored in a dark place, so that the titanium dioxide/aminated graphene quantum dot composite material is prepared;
step 2: the prepared titanium dioxide/aminated graphene quantum dot composite material is coated on a photonic crystal fiber to form a detection film. The process specifically comprises the following steps: fixing the photonic crystal fiber section in a suspended state, then placing the fixed photonic crystal fiber section into a vacuum drying oven for drying treatment, taking the optical fiber crystal fiber with the length of 7cm after drying, removing a coating layer by using an optical fiber wire stripper, and cleaning the optical fiber crystal fiber; the photonic crystal fiber section is fixed in a suspended state and is dried, so that the condition of uneven film formation caused by horizontal placement is prevented; in addition, the adhesive force between the graphene material and the photonic crystal fiber section can be further enhanced in the calcining process, so that the graphene material becomes a stable film structure, and the structure of the photonic crystal fiber section cannot be damaged.
Putting the sheared photonic crystal fiber on a clean glass slide, taking the prepared titanium dioxide/aminated graphene quantum dot solution by using a pipette, dropwise adding the solution on the fiber, dip-coating for 10 minutes, and taking out, wherein the steps are repeatedly carried out for a plurality of times, preferably for four times;
placing the glass slide with the photonic crystal fiber in a vacuum drying box for drying; drying at the optimal drying temperature of 300 ℃ for 2 hours to form the photonic crystal fiber coated with the titanium dioxide/aminated graphene quantum dot composite material;
and step 3: cutting two ends of the coated photonic crystal fiber by using a fiber cutter, keeping the length of the photonic crystal fiber at 4.5cm, respectively welding two ends of the cut section with a section of multimode fiber in a tapering welding manner by using an optical fiber welding machine, and then respectively welding two sections of multimode fiber with a section of single-mode fiber; wherein, the photonic crystal fiber is far away from the electrode during welding, and two times of discharge are carried out; after the first discharge, the edges at the welding points are firstly welded, and the air discharged from the center due to the collapse of the air holes of the cladding of the photonic crystal fiber is captured to form an air cavity; the reflection spectrum is monitored in real time, and discharge is added for multiple times, so that the fineness and the contrast of the reflection stripes are maximized. After the end face of the optical fiber is melted, aligning the photonic crystal fiber and the first multimode fiber, advancing the photonic crystal fiber and the first multimode fiber by a preset length, and then drawing the photonic crystal fiber and the first multimode fiber back to complete the fusion splicing of the photonic crystal fiber and the first multimode fiber; and repeating the steps on the other end face of the photonic crystal fiber and the second multimode fiber until the stretching distance reaches a preset value. In order to ensure that the optical fiber fusion splice has low loss and achieves the best fusion splice effect, except that the tail end of the optical fiber is clean and stripped, different optical fibers should select proper fusion splice procedures before fusion splice. It is guaranteed that no bubble exists at the welding position, a collapse layer can be formed, and no miscellaneous peak appears in interference spectrum, so that part of light transmitted by the single-mode fiber can enter a cladding of the photonic crystal fiber at the welding position to form two beams of light, and the interference condition is met. The tapering method provided by this embodiment can make the core and the cladding light interfere better by lengthening the length of the collapse layer, and the interference intensity and the spectral shift thereof will increase accordingly.
Photonic crystal fibers with different lengths are built into a Mach-Zehnder interference structure, and the number of interference wave peaks and interference peaks is observed through a spectrometer to confirm that the optimal interference effect can be found, so that the optimal length of the photonic crystal fiber of the gas sensor can be found. In the sensing structure, the longer the length of the photonic crystal fiber is, the more the number of the obtained interference peaks is, that is, the denser the interference peaks are, the shorter the length of the photonic crystal fiber is, the obviously reduced number of the obtained interference peaks is, and even the unsmooth peaks appear. The invention comprehensively considers the characteristics of proper wave crest quantity and less curve smooth burrs, and selects the optimal length of the photonic crystal fiber to be 4.5 cm.
The optical fiber hydrogen sulfide gas sensor prepared by the method detects hydrogen sulfide with different concentrations, such as H with the detected concentrations of 10ppm, 20ppm, 30ppm, 40ppm, 50ppm and 55ppm respectively2And S gas, collecting spectrograms of the hydrogen sulfide gas under different concentrations through a spectrometer, selecting the central wavelength of the same peak in the spectrograms, and obtaining p which is m-nc through linear fitting, namely c which is (m-p)/n, wherein p is the central wavelength of the peak in the detection spectrum of the hydrogen sulfide gas chamber, m is the central wavelength of the peak in the detection spectrum without containing the hydrogen sulfide gas, n is the offset of every 1ppm of the hydrogen sulfide gas in the spectrum and the sensitivity of the sensor, and c is the concentration of the hydrogen sulfide gas. As shown in FIG. 1, a peak at 1538.9nm in the output spectrum is selected for monitoring, the deviation condition of the peak along with the concentration of H2S gas within the range of 0-55 ppm is tested, and the output spectrum shows an obvious blue shift phenomenon along with the increase of the concentration of H2S gas. The titanium dioxide/aminated graphene quantum dot sensitive film in the sensing area adsorbs H2S gas molecules increase the refractive index of the cladding, so that the fiber core and the claddingThe difference between the effective refractive indices of the layers is increased, so that the center wavelength is blue-shifted, and the experimental result is consistent with the theoretical analysis. The sensitivity of the sensor to hydrogen sulfide was calculated to be 26.62pm/ppm and the linearity was 0.99249 by means of the above linear fit over the range of 0-55pp hydrogen sulfide concentrations. The experimental result shows that the sensor pair H2S has high selectivity.
It is to be noted that the foregoing is only illustrative of the preferred embodiments of the present invention and the technical principles employed. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, but is capable of various obvious changes, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, although the present invention has been described in greater detail by the above embodiments, the present invention is not limited to the above embodiments, and may include other equivalent embodiments without departing from the spirit of the present invention, and the scope of the present invention is determined by the scope of the appended claims.
Claims (3)
1. A preparation method of an optical fiber gas sensor comprises a first single mode optical fiber, a first multimode optical fiber, a photonic crystal optical fiber, a second multimode optical fiber and a second single mode optical fiber, wherein two ends of the photonic crystal optical fiber are respectively connected with the first multimode optical fiber and the second multimode optical fiber, the two ends of the first multimode optical fiber and the second multimode optical fiber are respectively welded with the first single mode optical fiber and the second single mode optical fiber, and the surface of the photonic crystal optical fiber is coated with a titanium dioxide/aminated graphene quantum dot composite sensitive film; the method specifically comprises the following steps:
step 1: preparing a titanium dioxide/aminated graphene quantum dot composite material solution;
step 2: coating the prepared titanium dioxide/aminated graphene quantum dot composite material on a photonic crystal fiber to form a detection film;
and step 3: cutting two ends of the coated photonic crystal fiber by using a fiber cutter, keeping the length of the photonic crystal fiber at 4.5cm, respectively welding two ends of the cut section with a section of multimode fiber in a tapering welding manner by using an optical fiber welding machine, and then respectively welding two sections of multimode fiber with a section of single-mode fiber;
wherein, with the optical fiber splicer with cut the both ends of section through the mode of tapering butt fusion respectively with one section multimode fiber splice, specifically include:
the photonic crystal fiber is far away from the electrode, and two times of discharge are carried out; after the first discharge, the edges at the welding points are firstly welded, and the air discharged from the center due to the collapse of the air holes of the cladding of the photonic crystal fiber is captured to form an air cavity;
after the end face of the optical fiber is melted, aligning the photonic crystal fiber and the first multimode fiber, advancing the photonic crystal fiber and the first multimode fiber by a preset length, and then drawing the photonic crystal fiber and the first multimode fiber back to complete the fusion splicing of the photonic crystal fiber and the first multimode fiber; and repeating the steps on the other end face of the photonic crystal fiber and the second multimode fiber until the stretching distance reaches a preset value.
2. The method for manufacturing the optical fiber gas sensor according to claim 1, wherein the step 1 is specifically: weighing 0.04g of nano titanium dioxide with the particle size of 5-10nm by using an electronic balance, dispersing the nano titanium dioxide in 50ml of deionized water, preparing a nano titanium dioxide aqueous solution, adding a stirrer, and covering a preservative film;
stirring the mixed solution on a constant-temperature heating magnetic stirrer, taking 1ml of the mixed solution in a small test tube by using a pipette, taking 1ml of aminated graphene quantum dots with the concentration of 1mg/ml and the particle size of 2.5-4.5nm, mixing the aminated graphene quantum dots with the aminated graphene quantum dots, and putting the mixture in a mechanical ultrasonic cleaning machine for treatment; in the ultrasonic mixing process, the temperature is controlled to be lower than 4 ℃, and ultrasonic treatment is carried out for 20 minutes.
3. The method for manufacturing the optical fiber gas sensor according to claim 1, wherein the step 2 is specifically: fixing the photonic crystal fiber section in a suspended state, then placing the fixed photonic crystal fiber section into a vacuum drying oven for drying treatment, taking the optical fiber crystal fiber with the length of 7cm after drying, removing a coating layer by using an optical fiber wire stripper, and cleaning the optical fiber crystal fiber; putting the sheared photonic crystal fiber on a clean glass slide, taking the prepared titanium dioxide/aminated graphene quantum dot solution by using a pipette, dropwise adding the solution on the fiber, taking out after dip-coating for 10 minutes, and repeating the steps for many times; placing the glass slide with the photonic crystal fiber in a vacuum drying box for drying; wherein the optimum drying temperature is 300 ℃ for 2 hours.
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