CN111121963A - Rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor and manufacturing method thereof - Google Patents
Rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor and manufacturing method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 70
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- 239000013307 optical fiber Substances 0.000 claims abstract description 108
- 239000000463 material Substances 0.000 claims abstract description 39
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 25
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 25
- 239000002184 metal Substances 0.000 claims abstract description 25
- 239000000835 fiber Substances 0.000 claims description 62
- 238000002360 preparation method Methods 0.000 claims description 16
- 239000002121 nanofiber Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 230000004927 fusion Effects 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
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- 239000000725 suspension Substances 0.000 claims description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
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- 210000004705 lumbosacral region Anatomy 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 10
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J1/00—Photometry, e.g. photographic exposure meter
- G01J1/42—Photometry, e.g. photographic exposure meter using electric radiation detectors
- G01J1/429—Photometry, e.g. photographic exposure meter using electric radiation detectors applied to measurement of ultraviolet light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J1/00—Photometry, e.g. photographic exposure meter
- G01J1/02—Details
- G01J1/04—Optical or mechanical part supplementary adjustable parts
- G01J1/0407—Optical elements not provided otherwise, e.g. manifolds, windows, holograms, gratings
- G01J1/0425—Optical elements not provided otherwise, e.g. manifolds, windows, holograms, gratings using optical fibers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/02—Details
- G01J3/0205—Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows
- G01J3/0218—Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows using optical fibers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/28—Investigating the spectrum
- G01J3/45—Interferometric spectrometry
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Abstract
The invention discloses a rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor and a manufacturing method thereof, and belongs to the field of optical fiber sensing. The ultraviolet sensor comprises an ASE light source, an optical fiber circulator, an ultraviolet sensing head and a spectrometer. The signal light is transmitted to the ultraviolet sensing head through the optical fiber circulator by the ASE light source, the signal light is reflected by the metal aluminum film in the ultraviolet sensing head, passes through the single-mode-tapered multi-mode-single-mode optical fiber structure for the second time, forms strong interference by means of the single-sphere micro-nano structure, is transmitted outwards in a basic mode, and finally is transmitted to the spectrometer through the optical fiber circulator by the ultraviolet sensing head. The sensor has the advantage that the interference spectrum of the sensor is greatly drifted due to ultraviolet change by means of the prepared rod-shaped ZnO/graphene ultraviolet sensitive material and the strong interference optical fiber structure. The corresponding uv change can be measured by the amount of drift. The invention combines the sensitive material and the special interference type optical fiber structure, so that the optical fiber ultraviolet sensor successfully realizes the superior performances of high sensitivity, strong stability and low cost.
Description
Technical Field
The invention belongs to the technical field of optical fiber sensors, and particularly relates to a rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor and a manufacturing method thereof.
Technical Field
Ultraviolet detection is spread in all corners of people's life, and optical fiber ultraviolet sensors are widely used as the last-generation ultraviolet sensors in the category of ultraviolet sensors by virtue of the advantages of small size, corrosion resistance, high temperature resistance and strong electromagnetic interference resistance. However, with the development and progress of production and life, the sensitive performance of the sensor is required to be higher and higher.
The improvement on the optical fiber structure can well improve the sensitivity of the sensor. In recent years, an optical fiber sensor formed by combining a sensitive material as a sensing medium and an optical fiber structure has been developed in the aspects of sensitivity, stability and the like. Such fiber optic sensors are becoming increasingly favored with a number of advantages, also in the context of uv sensing. Therefore, the optical fiber ultraviolet sensor has the advantages that the optical fiber ultraviolet sensor is combined with a special optical fiber structure with a strong interference effect, sensitive materials with better selectivity can be selected, the ultraviolet photosensitive performance of the optical fiber ultraviolet sensor is improved, and the optical fiber ultraviolet sensor has important significance in better solving the ultraviolet detection problem in different severe environments.
Disclosure of Invention
Aiming at the defects and improvement needs of the prior art, the invention provides a rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor and a manufacturing method thereof, and aims to combine a sensitive material preparation method, fuse a novel composite sensitive material with a special optical fiber structure with a strong interference effect, and prepare the optical fiber ultraviolet sensor with high sensitivity, strong stability and low cost by means of the ultraviolet photosensitive property of the rod-shaped ZnO/graphene material, so that the ultraviolet detection problem in severe environments is better solved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized by comprising an ASE light source (1), an optical fiber circulator (2), an ultraviolet sensing head (3) and a spectrometer (4).
The ultraviolet sensing head (3) comprises a first single mode fiber (3-1), a multimode single sphere micro-nano fiber (3-2), a rod-shaped ZnO/graphene sensitive material (3-3), a second single mode fiber (3-4) and a metal aluminum film (3-5).
The ultraviolet sensing head (3) takes a multimode single-sphere micro-nano optical fiber (3-2) as a main ultraviolet photosensitive area, the multimode single-sphere micro-nano optical fiber (3-2) coats a rod-shaped ZnO/graphene sensitive material (3-3) with better ultraviolet photosensitive performance, and is connected with a first single-mode optical fiber (3-1) and a second single-mode optical fiber (3-4) in an optical fiber fusion connection mode.
In the ultraviolet sensing head (3), one end of a second single-mode fiber (3-4) is connected with the multimode single-sphere micro-nano fiber (3-2) in a melting mode, and the other end of the second single-mode fiber is coated with a metal aluminum film (3-5).
The ASE light source (1) is connected with the optical fiber circulator (2) through a single-mode optical fiber, the optical fiber circulator (2) is connected with the ultraviolet sensing head (3) through the single-mode optical fiber, the optical fiber circulator (2) is connected with the spectrometer (4) through the single-mode optical fiber, and the single-mode optical fiber is connected with each device in an optical fiber fusion connection mode.
The rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized in that the output center wavelength of the ASE light source (1) is 1550nm, and the frequency bandwidth is 60 nm.
The rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized in that a rod-shaped ZnO/graphene sensitive material (3-3) in the ultraviolet sensing head (3) is an ultraviolet composite sensitive material.
The ultraviolet sensor with the rod-shaped ZnO/graphene single-sphere micro-nano structure is characterized in that a method for combining the multimode single-sphere micro-nano optical fiber (3-2) with the rod-shaped ZnO/graphene sensitive material (3-3) in the ultraviolet sensing head (3) is a dripping method.
The preparation method of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized by comprising the following steps:
s1: preparing a multimode single-sphere micro-nano optical fiber (3-2), namely performing oxyhydrogen flame melting tapering treatment on the multimode optical fiber with the length of 8cm and the fiber core diameter of 62.5 mu m to prepare the multimode single-sphere micro-nano optical fiber (3-2);
s2: preparing a rodlike ZnO/graphene sensitive material (3-3), namely placing 6.0mg of graphene powder into 20mL of deionized water for ultrasonic dispersion for 1.5h, mixing the dispersed graphene solution with 0.7g of zinc nitrate and 60mL of deionized water, stirring at 28 ℃, dripping 1mol/L sodium hydroxide solution into the mixed solution, adjusting the pH value of the suspension to 7.8, continuing stirring for 1.5-2h, transferring the suspension into a reaction kettle, placing the reaction kettle into a 130 ℃ constant-temperature drying box for 20h, taking out, naturally cooling, washing the product with the deionized water for 4-5 times, and centrifuging for 15min at 5000rmp/min to obtain a rodlike ZnO/graphene aqueous solution;
s3: preparing a single mode-tapering multi-mode-single mode fiber structure, intercepting two single mode fibers with the length of 5cm as a first single mode fiber (3-1) and a second single mode fiber (3-4), and connecting the first single mode fiber (3-1), the multi-mode single-sphere micro-nano fiber (3-2) and the second single mode fiber (3-4) in a fiber fusion connection mode to form the single mode-tapering multi-mode-single mode fiber structure;
s4: cladding of the metal aluminum film (3-5), namely truncating the end, which is not welded, of the second single-mode fiber (3-4) in the single-mode-tapered multi-mode-single-mode fiber structure, and cladding the metal aluminum film (2) with better reflection performance on the end;
s5: and (3) integrating an ultraviolet sensing head (3), fixing a single-mode-tapered multi-mode-single-mode optical fiber structure which is manufactured but is not coated with a material in a dripping mode on a glass substrate, cleaning the glass substrate by using alcohol and deionized water to remove residual impurities, dripping a rod-shaped ZnO/graphene aqueous solution along the surface of the multi-mode single-sphere micro-nano optical fiber (3-2), and putting the sensing head into a constant-temperature electrothermal blowing drying box for drying treatment to enable the sensitive material to be tightly combined with the multi-mode single-sphere micro-nano optical fiber (3-2) to form the ultraviolet sensing head (3).
The preparation method of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized in that oxyhydrogen flame melting tapering is carried out in the step S1, a oxyhydrogen flame tapering machine is adopted to carry out melting tapering for 12.4mm, a multimode micro-nano optical fiber with the lumbar vertebra diameter of 6.92 mu m is formed, a clamp is adjusted back for 1mm, the multimode micro-nano optical fiber lumbar vertebra region is burned and melted by oxyhydrogen flame, a multimode single-sphere micro-nano optical fiber (3-2) is formed, and the diameter of a single sphere is 13.1 mu m.
The preparation method of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized in that in the step S4 of coating the metal aluminum film (3-5), the length of the second single-mode optical fiber (3-4) after being truncated is 3 cm.
The preparation method of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized in that in the step S4 of coating the metal aluminum film (3-5), the thickness of the metal aluminum film (2) can be 80-200 mu m.
The preparation method of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized in that in the step S5 of integrating the ultraviolet sensing head (3), the temperature of the constant-temperature electrothermal blowing drying oven is set to be 45 ℃, and the heating time is 5 hours.
The beneficial effects of the invention are as follows:
the invention combines the preparation method of the sensitive material, fuses the novel composite sensitive material with a special optical fiber structure with a strong interference effect, and prepares the optical fiber ultraviolet sensor with high sensitivity, strong stability and low cost by means of the ultraviolet photosensitive property of the rod-shaped ZnO/graphene material. The method has important significance for better solving the ultraviolet detection problem in severe environments.
Drawings
FIG. 1 is a schematic structural diagram of a rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor;
FIG. 2 is a block diagram of an ultraviolet sensor head;
FIG. 3 is a drift diagram of an interference spectrum of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor under different ultraviolet light intensities;
FIG. 4 is a data fitting graph of interference spectra in an ultraviolet detection experiment;
FIG. 5 is a flow chart of a method of fabricating an ultraviolet sensing head;
FIG. 6 is an SEM image of the rod-shaped ZnO/graphene prepared by the invention.
Detailed Description
The following description will further describe the specific embodiments of the present invention with reference to the accompanying drawings.
Referring to fig. 1, the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor according to the embodiment is characterized by comprising an ASE light source (1), an optical fiber circulator (2), an ultraviolet sensing head (3) and a spectrometer (4).
Referring to fig. 2, the ultraviolet sensing head (3) comprises a first single mode fiber (3-1), a multimode single sphere micro-nano fiber (3-2), a rod-shaped ZnO/graphene sensitive material (3-3), a second single mode fiber (3-4) and a metal aluminum film (3-5).
The ultraviolet sensing head (3) takes a multimode single-sphere micro-nano optical fiber (3-2) as a main ultraviolet photosensitive area, the multimode single-sphere micro-nano optical fiber (3-2) coats a rod-shaped ZnO/graphene sensitive material (3-3) with better ultraviolet photosensitive performance, and is connected with a first single-mode optical fiber (3-1) and a second single-mode optical fiber (3-4) in an optical fiber fusion connection mode.
In the ultraviolet sensing head (3), one end of a second single-mode fiber (3-4) is connected with the multimode single-sphere micro-nano fiber (3-2) in a melting mode, and the other end of the second single-mode fiber is coated with a metal aluminum film (3-5).
The ASE light source (1) is connected with the optical fiber circulator (2) through a single-mode optical fiber, the optical fiber circulator (2) is connected with the ultraviolet sensing head (3) through the single-mode optical fiber, the optical fiber circulator (2) is connected with the spectrometer (4) through the single-mode optical fiber, and the single-mode optical fiber is connected with each device in an optical fiber fusion connection mode.
The rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized in that the output center wavelength of the ASE light source (1) is 1550nm, and the frequency bandwidth is 60 nm.
The rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized in that a rod-shaped ZnO/graphene sensitive material (3-3) in the ultraviolet sensing head (3) is an ultraviolet composite sensitive material.
The ultraviolet sensor with the rod-shaped ZnO/graphene single-sphere micro-nano structure is characterized in that a method for combining the multimode single-sphere micro-nano optical fiber (3-2) with the rod-shaped ZnO/graphene sensitive material (3-3) in the ultraviolet sensing head (3) is a dripping method.
The preparation method of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized by comprising the following steps:
s1: preparing a multimode single-sphere micro-nano optical fiber (3-2), namely performing oxyhydrogen flame melting tapering treatment on the multimode optical fiber with the length of 8cm and the fiber core diameter of 62.5 mu m to prepare the multimode single-sphere micro-nano optical fiber (3-2);
s2: preparing a rodlike ZnO/graphene sensitive material (3-3), namely placing 6.0mg of graphene powder into 20mL of deionized water for ultrasonic dispersion for 1.5h, mixing the dispersed graphene solution with 0.7g of zinc nitrate and 60mL of deionized water, stirring at 28 ℃, dripping 1mol/L sodium hydroxide solution into the mixed solution, adjusting the pH value of the suspension to 7.8, continuing stirring for 1.5-2h, transferring the suspension into a reaction kettle, placing the reaction kettle into a 130 ℃ constant-temperature drying box for 20h, taking out, naturally cooling, washing the product with the deionized water for 4-5 times, and centrifuging for 15min at 5000rmp/min to obtain a rodlike ZnO/graphene aqueous solution;
s3: preparing a single mode-tapering multi-mode-single mode fiber structure, intercepting two single mode fibers with the length of 5cm as a first single mode fiber (3-1) and a second single mode fiber (3-4), and connecting the first single mode fiber (3-1), the multi-mode single-sphere micro-nano fiber (3-2) and the second single mode fiber (3-4) in a fiber fusion connection mode to form the single mode-tapering multi-mode-single mode fiber structure;
s4: cladding of the metal aluminum film (3-5), namely truncating the end, which is not welded, of the second single-mode fiber (3-4) in the single-mode-tapered multi-mode-single-mode fiber structure, and cladding the metal aluminum film (2) with better reflection performance on the end;
s5: and (3) integrating an ultraviolet sensing head (3), fixing a single-mode-tapered multi-mode-single-mode optical fiber structure which is manufactured but is not coated with a material in a dripping mode on a glass substrate, cleaning the glass substrate by using alcohol and deionized water to remove residual impurities, dripping a rod-shaped ZnO/graphene aqueous solution along the surface of the multi-mode single-sphere micro-nano optical fiber (3-2), and putting the sensing head into a constant-temperature electrothermal blowing drying box for drying treatment to enable the sensitive material to be tightly combined with the multi-mode single-sphere micro-nano optical fiber (3-2) to form the ultraviolet sensing head (3).
The preparation method of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized in that oxyhydrogen flame melting tapering is carried out in the step S1, a oxyhydrogen flame tapering machine is adopted to carry out melting tapering for 12.4mm, a multimode micro-nano optical fiber with the lumbar vertebra diameter of 6.92 mu m is formed, a clamp is adjusted back for 1mm, the multimode micro-nano optical fiber lumbar vertebra region is burned and melted by oxyhydrogen flame, a multimode single-sphere micro-nano optical fiber (3-2) is formed, and the diameter of a single sphere is 13.1 mu m.
The preparation method of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized in that in the step S4 of coating the metal aluminum film (3-5), the length of the second single-mode optical fiber (3-4) after being truncated is 3 cm.
The preparation method of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized in that in the step S4 of coating the metal aluminum film (3-5), the thickness of the metal aluminum film (2) can be 80-200 mu m.
The preparation method of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized in that in the step S5 of integrating the ultraviolet sensing head (3), the temperature of the constant-temperature electrothermal blowing drying oven is set to be 45 ℃, and the heating time is 5 hours.
The working principle is as follows:
ultraviolet sensor of rod-like ZnO/graphene single sphere micro-nano structure:
the working process is as follows: signal light is transmitted to an ultraviolet sensing head (3) from an ASE light source (1) along a single mode fiber through a fiber circulator (2), in the ultraviolet sensing head (3), the signal light is transmitted to a multimode single sphere micro-nano fiber (3-2) through a first single mode fiber (3-1), then transmitted to a second single mode fiber (3-3) through the multimode single sphere micro-nano fiber (3-2), reflected at a metal aluminum film (3-5) through the second single mode fiber (3-3), and then sequentially passes through the second single mode fiber (3-3), the multimode single sphere micro-nano fiber (3-2) and the first single mode fiber (3-1), and finally transmitted to a spectrometer (4) from the ultraviolet sensing head (3) through the fiber circulator (2).
In the process of signal light transmission, the diameter of the fiber core of the multimode fiber is far larger than that of the common single-mode fiber, the fiber core of the multimode fiber can accommodate various light wave modes, and multimode interference effect can occur in different modes in the transmission process. In addition, the surface evanescent field of the multimode single-sphere micro-nano optical fiber after tapering and ball melting treatment is enhanced, the interaction between light and the external environment is increased when the light is transmitted in the multimode single-sphere micro-nano optical fiber, and particularly the interference effect in a single sphere is better. When signal light passes through the ultraviolet sensing head (3), a series of mutually independent eigen modes can be excited by the single mode fiber (3-1) to the multimode single sphere micro-nano fiber (3-2), each mode interferes in the fiber, energy redistribution can be generated, and optical coupling is formed when the signal light is transmitted to the second single mode fiber (3-3) again through the multimode single sphere micro-nano fiber (3-2) and transmitted in a mode of a fundamental mode. When the signal light reaches the metal aluminum film (3-5), the signal light is reflected and passes through the optical fiber structure formed by combining the second single-mode optical fiber (3-3), the multi-mode single-sphere micro-nano optical fiber (3-2) and the first single-mode optical fiber (3-1) again to form secondary interference, and finally the signal light is transmitted to the circulator from the first single-mode optical fiber (3-1) in a basic mode.
The difference in refractive index between the different modes is Δ n, the phase difference can be expressed as:
considering the inter-mode dispersion, the wavelength shift and external index relationship can be expressed as:
the dispersion factor is:
thus, the sensitivity of the UV sensor depends on the difference in effective refractive index and the dispersion factor between the modes. The invention adopts the multimode single-sphere micro-nano optical fiber (3-2), which has stronger sensitivity to the change of the external refractive index due to stronger evanescent field and smaller dispersion factor. In addition, the rod-shaped ZnO/graphene sensitive material (3-3) selected and prepared by the invention is very sensitive to ultraviolet light, and the structure of the material can be changed to a great extent by changing the intensity of the ultraviolet light, so that the refractive index of the material is changed. The multimode single-sphere micro-nano optical fiber (3-2) is compounded with the rod-shaped ZnO/graphene sensitive material (3-3), and the single mode-tapered multimode-single mode and the metal aluminum film (3-5) are combined to enable signal light to form secondary interference, so that the ultraviolet photosensitivity of the ultraviolet sensing head (3) is greatly enhanced, and the ultraviolet sensor has high sensitivity and stability.
The effect of the invention is demonstrated by the following examples:
an ultraviolet sensing head (3) of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is placed under an ultraviolet lamp for irradiation, when ultraviolet illumination is changed, the effective refractive index of the optical fiber of the sensing part is changed by combining the multi-mode single-sphere micro-nano optical fiber (3-2) and the rod-shaped ZnO/graphene sensitive material (3-3), and the interference spectrum is obviously and regularly drifted along with the change of the ultraviolet illumination. FIG. 3 shows the drift of the interference spectrum of the UV sensor under different UV intensities, wherein the UV intensity represented by the curve in the direction of the arrow in the figure is 0nW/cm from top to bottom2、0.895nW/cm2、1.362nW/cm2、1.829nW/cm2、2.296nW/cm2、2.763nW/cm2、3.23nW/cm2、3.697nW/cm2、4.164nW/cm2. Fig. 4 is a data fitting graph of interference spectrum in the uv experiment, and the selected data points are peaks and peaks of the interference spectrum under different uv within the dashed box in fig. 3, where the slope is 0.24813 and the goodness of fit is 0.99363.
As can be seen from fig. 4, as the ultraviolet irradiation intensity increases, the ultraviolet sensor interference spectrum shifts with a clear regularity. In addition, the sensitivity of the sensor to ultraviolet can be obtained by processing data of interference spectrum drift amount and ultraviolet change in an ultraviolet experiment, and the sensitivity can reach 248.13pm/(nW cm)-2)。
Claims (9)
1. The rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor is characterized by comprising an ASE light source (1), an optical fiber circulator (2), an ultraviolet sensing head (3) and a spectrometer (4);
the ultraviolet sensing head (3) comprises a first single mode fiber (3-1), a multimode single sphere micro-nano fiber (3-2), a rod-shaped ZnO/graphene sensitive material (3-3), a second single mode fiber (3-4) and a metal aluminum film (3-5);
the ultraviolet sensing head (3) takes a multimode single-sphere micro-nano optical fiber (3-2) as a main ultraviolet photosensitive area, the multimode single-sphere micro-nano optical fiber (3-2) coats a rod-shaped ZnO/graphene sensitive material (3-3) with better ultraviolet photosensitive performance, and is connected with a first single-mode optical fiber (3-1) and a second single-mode optical fiber (3-4) in an optical fiber fusion connection mode;
in the ultraviolet sensing head (3), one end of a second single-mode fiber (3-4) is connected with the multimode single-sphere micro-nano fiber (3-2) in a melting way, and the other end of the second single-mode fiber is coated with a metal aluminum film (3-5);
the ASE light source (1) is connected with the optical fiber circulator (2) through a single-mode optical fiber, the optical fiber circulator (2) is connected with the ultraviolet sensing head (3) through the single-mode optical fiber, the optical fiber circulator (2) is connected with the spectrometer (4) through the single-mode optical fiber, and the single-mode optical fiber is connected with each device in an optical fiber fusion connection mode.
2. The ultraviolet sensor with the rod-shaped ZnO/graphene single-sphere micro-nano structure according to claim 1, wherein the output center wavelength of the ASE light source (1) is 1550nm, and the frequency bandwidth is 60 nm.
3. The ultraviolet sensor with the rod-shaped ZnO/graphene single-sphere micro-nano structure according to claim 1, wherein a rod-shaped ZnO/graphene sensitive material (3-3) in the ultraviolet sensing head (3) is an ultraviolet composite sensitive material.
4. The ultraviolet sensor with the rod-shaped ZnO/graphene single-sphere micro-nano structure according to claim 1, wherein a method for combining the multimode single-sphere micro-nano optical fiber (3-2) with the rod-shaped ZnO/graphene sensitive material (3-3) in the ultraviolet sensing head (3) is a dropping coating method.
5. The preparation method of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor according to claim 1, which is characterized by comprising the following steps:
s1: preparing a multimode single-sphere micro-nano optical fiber (3-2), namely performing oxyhydrogen flame melting tapering treatment on the multimode optical fiber with the length of 8cm and the fiber core diameter of 62.5 mu m to prepare the multimode single-sphere micro-nano optical fiber (3-2);
s2: preparing a rodlike ZnO/graphene sensitive material (3-3), namely placing 6.0mg of graphene powder into 20mL of deionized water for ultrasonic dispersion for 1.5h, mixing the dispersed graphene solution with 0.7g of zinc nitrate and 60mL of deionized water, stirring at 28 ℃, dripping 1mol/L sodium hydroxide solution into the mixed solution, adjusting the pH value of the suspension to 7.8, continuing stirring for 1.5-2h, transferring the suspension into a reaction kettle, placing the reaction kettle into a 130 ℃ constant-temperature drying box for 20h, taking out, naturally cooling, washing the product with the deionized water for 4-5 times, and centrifuging for 15min at 5000rmp/min to obtain a rodlike ZnO/graphene aqueous solution;
s3: preparing a single mode-tapering multi-mode-single mode fiber structure, intercepting two single mode fibers with the length of 5cm as a first single mode fiber (3-1) and a second single mode fiber (3-4), and connecting the first single mode fiber (3-1), the multi-mode single-sphere micro-nano fiber (3-2) and the second single mode fiber (3-4) in a fiber fusion connection mode to form the single mode-tapering multi-mode-single mode fiber structure;
s4: cladding of the metal aluminum film (3-5), namely truncating the end, which is not welded, of the second single-mode fiber (3-4) in the single-mode-tapered multi-mode-single-mode fiber structure, and cladding the metal aluminum film (2) with better reflection performance on the end;
s5: and (3) integrating an ultraviolet sensing head (3), fixing a single-mode-tapered multi-mode-single-mode optical fiber structure which is manufactured but is not coated with a material in a dripping mode on a glass substrate, cleaning the glass substrate by using alcohol and deionized water to remove residual impurities, dripping a rod-shaped ZnO/graphene aqueous solution along the surface of the multi-mode single-sphere micro-nano optical fiber (3-2), and putting the sensing head into a constant-temperature electrothermal blowing drying box for drying treatment to enable the sensitive material to be tightly combined with the multi-mode single-sphere micro-nano optical fiber (3-2) to form the ultraviolet sensing head (3).
6. The preparation method of the ultraviolet sensor with the rod-shaped ZnO/graphene single-sphere micro-nano structure according to claim 5, wherein oxyhydrogen flame is used for fusion tapering in step S1, a oxyhydrogen flame tapering machine is used for fusion tapering by 12.4mm to form the multimode micro-nano optical fiber with the lumbar diameter of 6.92 microns, a clamp is adjusted back by 1mm, the multimode micro-nano optical fiber is burned and melted in the lumbar region through oxyhydrogen flame to form the multimode single-sphere micro-nano optical fiber (3-2), and the diameter of the single sphere is 13.1 microns.
7. The preparation method of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor according to claim 5, wherein in the coating of the metal aluminum film (3-5) in the step S4, the length of the second single-mode optical fiber (3-4) after being truncated is 3 cm.
8. The method for preparing the ultraviolet sensor with the rod-shaped ZnO/graphene single-sphere micro-nano structure according to claim 5, wherein in the step S4 of coating the metal aluminum film (3-5), the thickness of the metal aluminum film (2) can be 80-200 μm.
9. The preparation method of the rod-shaped ZnO/graphene single-sphere micro-nano structure ultraviolet sensor according to claim 5, wherein in the integration of the ultraviolet sensor head (3) in the step S5, the temperature of a constant temperature electrothermal blowing dry box is set to be 45 ℃, and the heating time is 5 hours.
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| CN103884364A (en) * | 2014-04-18 | 2014-06-25 | 天津理工大学 | Optical fiber interferometric sensor based on cascade connection between tapered structure and spherical structure |
| CN206684285U (en) * | 2017-04-12 | 2017-11-28 | 中国计量大学 | A kind of magnetic field sensor based on shaddock type optical fiber and bragg grating |
| CN110672135A (en) * | 2019-11-18 | 2020-01-10 | 哈尔滨理工大学 | Fiber bragg grating ultraviolet sensing method and device capable of compensating temperature |
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| CN103884364A (en) * | 2014-04-18 | 2014-06-25 | 天津理工大学 | Optical fiber interferometric sensor based on cascade connection between tapered structure and spherical structure |
| CN206684285U (en) * | 2017-04-12 | 2017-11-28 | 中国计量大学 | A kind of magnetic field sensor based on shaddock type optical fiber and bragg grating |
| CN110672135A (en) * | 2019-11-18 | 2020-01-10 | 哈尔滨理工大学 | Fiber bragg grating ultraviolet sensing method and device capable of compensating temperature |
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| CN112432912A (en) * | 2020-11-19 | 2021-03-02 | 哈尔滨理工大学 | Optical fiber ultraviolet sensing device based on interference array and implementation method |
| CN112432912B (en) * | 2020-11-19 | 2021-09-24 | 哈尔滨理工大学 | Optical fiber ultraviolet sensing device based on interference array and implementation method |
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