CN109655159B - Based on Al2O3Optical fiber ultraviolet sensor of/ZnO and manufacturing method thereof - Google Patents
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000013307 optical fiber Substances 0.000 claims abstract description 142
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 22
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- 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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- 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
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Abstract
The invention discloses a catalyst based on Al2O3The optical fiber ultraviolet sensor of/ZnO comprises a plurality of optical fiber ultraviolet sensors which are connected in sequenceLight source, lead-in single mode fiber, first fine core fiber, hollow core fiber, Al2O3The optical fiber comprises/ZnO, a second fine-core optical fiber, an outgoing single-mode optical fiber and a spectrometer, wherein a light source of the optical fiber is a broadband light source, and the central wavelength of the optical fiber is 1550 nm; introducing a single mode optical fiber for receiving and transmitting light of a light source and transmitting it to a first thin core optical fiber; the first thin-core optical fiber is aligned with and welded with the introduced single-mode optical fiber to generate interference, and an interference signal mode is coupled to the hollow-core optical fiber; al is arranged in the hollow optical fiber2O3The two ends of the first fine-core optical fiber and the second fine-core optical fiber are in aligned fusion connection, and an interference signal is led out of the single-mode optical fiber to be output; the spectrometer performs spectral detection on the interference mode of the single-mode fiber and obtains sensing data. The invention also discloses a corresponding manufacturing method. According to the invention, by means of Al2O3the/ZnO enhances the absorptivity of ultraviolet, obviously improves the system sensitivity, and obtains the optical fiber ultraviolet sensor which is simple to manufacture and convenient to package.
Description
Technical Field
The invention belongs to the technical field of optical fiber sensors, and particularly relates to an Al-based optical fiber sensor2O3A ZnO optical fiber ultraviolet sensor and a manufacturing method thereof.
Background
Ultraviolet detection plays an important role in a wide range of civilian and military applications, including chemical and biological analysis, flame detection, satellite communications, transmitter calibration, and astronomical studies. Conventional uv detectors are implemented using photomultiplier tubes, which are fragile, bulky, heavy and costly. However, the wide bandgap semiconductor ZnO has received increasing attention from researchers, and as a unique photoelectric material, it has a significant band gap, high optical gain, and high transmittance in solar cells, lasers, transparent electrodes, and light emitting diodes. The optical fiber sensor has small volume, high temperature resistance, corrosion resistance and strong anti-electromagnetic interference capability, so that the defect that the traditional electrical sensor cannot work in environments of electromagnetic interference, high temperature and the like can be overcome.
The ZnO nano material has the characteristics of chemical stability, low toxicity, piezoelectricity and photoluminescence, and compared with the existing ultraviolet detection device, the optical fiber sensor is mainly a sensor manufactured by coating an optical fiber with the nano material, and the measurement of various parameters is realized at present, such as: temperature, magnetic field strength, concentration, etc. However, there are few reports on ultraviolet fiber sensors, and in the prior art, Azad et al ("Azad S, parviz R, Sadeghi e. side-detecting optical fiber coated with Zn (OH)2 nanoparticles for ultrasonic sensing applications", Laser Physics,2017,27(9):095901.) report on a fiber ultraviolet sensor based on Zn (OH)2 nanorods, that is, Zn (OH)2 nanorods are grown on a multimode micro-nano fiber by a chemical etching method, and this structure has a certain potential safety hazard in the process of manufacturing the micro-nano fiber, and can correspondingly cause the problems of low success rate, difficult packaging and the like of a fiber sensing device.
Disclosure of Invention
In response to the deficiencies and needs in the art, the present invention provides an Al based alloy2O3A ZnO optical fiber ultraviolet sensor and a manufacturing method thereof aim at effectively avoiding the problem of difficult packaging caused by manufacturing of a sensor cone by researching the interference property of an optical fiber and designing a sensitive component thereof, and Al is used2O3the/ZnO composite material enhances the ultraviolet absorption performance, so that the optical fiber ultraviolet sensor with high selectivity and high sensitivity is prepared.
According to one aspect of the present invention, there is provided an Al-based alloy2O3The optical fiber ultraviolet sensor of/ZnO is characterized by comprising a light source (1), a lead-in single mode optical fiber (2), a first thin core optical fiber (3), a hollow core optical fiber (4) and Al which are sequentially connected2O3The optical fiber comprises a/ZnO composite material (5), a second fine-core optical fiber (6), an outgoing single-mode optical fiber (7) and a spectrometer (8), wherein:
the light source (1) is a broadband light source, has a central wavelength of 1550nm and is used for generating optical signals;
the leading-in single-mode optical fiber (2) is used for receiving and transmitting the light of the light source (1) and transmitting the light to the first thin-core optical fiber (3);
the first thin-core optical fiber (3) is aligned and welded with the leading-in single-mode optical fiber (2) and used for generating interference and coupling the mode of an interference signal to the hollow-core optical fiber (4);
the hollow-core optical fiber (4) is internally provided with Al2O3The two ends of the/ZnO composite material (5) are respectively aligned and welded with the first fine-core optical fiber (3) and the second fine-core optical fiber (6), and an interference signal is output through the lead-out single-mode optical fiber (7);
and the spectrometer (8) executes transmission spectrum detection on the interference mode output by the leading-out single-mode fiber (7) and correspondingly obtains sensing data according to the detection structure.
Further preferably, the lengths of the first fine-core optical fiber (3) and the second fine-core optical fiber (6) are set to 1.5 cm.
As a further preference, Al grows in the hollow-core optical fiber (4)2O3The length of the/ZnO composite material (5) was set to 2 cm.
As a further preference, the Al grows in the hollow-core optical fiber (4)2O3The method of the/ZnO composite material (5) is as follows: growing the growth mixed solution in a reaction kettle at 200 ℃ for 20 hours by a hydrothermal method, washing the growth mixed solution for multiple times by deionized water, freeze-drying the growth mixed solution in vacuum for 24 hours, and calcining the powder of the growth mixed solution at 1200 ℃ for 3 hours to obtain Al2O3Powder, which is used as a raw material and is filled into ZnO solution prepared by a hydrothermal method by 1-5 percent, the cleaned hollow optical fiber (4) is immersed into 1-5 percent of mixed solution prepared by the hydrothermal method for growth for 10 hours at 100 ℃, and then drying treatment is carried out at 60 ℃ to ensure that Al is contained2O3the/ZnO composite material (5) grows in the hollow-core optical fiber (4) to form 350-400nm Al2O3the/ZnO composite material (5).
According to another aspect of the present invention, there is also provided a corresponding method for manufacturing a fiber-optic uv sensor, the method comprising the steps of:
(1) growing the growth mixed solution in a reaction kettle at 200 ℃ for 20 hours by a hydrothermal method, washing the growth mixed solution by deionized water mostly, freeze-drying the growth mixed solution in vacuum for 24 hours, and calcining the powder of the growth mixed solution at 1200 ℃ for 3 hours to obtain Al2O3Powder, which is used as a raw material and is filled into ZnO solution prepared by a hydrothermal method by 1 to 5 percent, the cleaned hollow-core optical fiber (4) is immersed into 1 to 5 percent of mixed solution prepared by the hydrothermal method for growth for 10 hours at 100 ℃, and then dried at 60 DEGTreatment of Al2O3the/ZnO composite material (5) grows in the hollow-core optical fiber (4) to form 350-400nm Al2O3a/ZnO composite material (5);
(2) the method comprises the steps that a user-defined mode of an optical fiber fusion splicer is adopted, the discharge intensity is adjusted to be 3500bit, the discharge time is 2000ms, one end of a single-mode fiber (2) is led in to be fused with a first thin-core fiber (3) in a fiber core alignment mode, then a hollow-core fiber (4) is continuously fused at the other end of the first thin-core fiber (3) in a fiber core alignment mode, then a second thin-core fiber (6) is fused at the other end of the hollow-core fiber (4) in a fiber core alignment mode, and finally a single-mode fiber (7) is led out in a fiber core alignment mode at the other end of the second thin-;
(3) and connecting the optical fiber element subjected to the welding with a light source (1) and a spectrometer (8), thereby completing the preparation process of the whole optical fiber ultraviolet sensor.
Further preferably, in the step (1), the length of the hollow-core optical fiber (4) is set to 2 cm.
Further preferably, in the step (2), the lengths of the first fine-core optical fiber (3) and the second fine-core optical fiber (6) are set to 1.5 cm.
In general, the Al-based alloy according to the invention2O3Compared with the prior art, the optical fiber ultraviolet sensor of/ZnO and the manufacturing method thereof mainly have the following technical advantages:
1. by adding the hollow-core optical fiber in the sensing element, the light energy can be concentrated at the edge part of the optical fiber as much as possible, and Al is added into the hollow-core optical fiber2O3the/ZnO composite material can obtain better ultraviolet sensing effect;
2. the designed sensor structure is a 5-segment structure, and thin-core optical fibers are introduced into two sides of a hollow optical fiber to form a sandwich structure, so that the coupling efficiency between the thin-core optical fibers and the hollow optical fiber can be changed;
3. the optical fiber sensor constructed according to the invention can complete the whole manufacturing process only by a hydrothermal method with a simple manufacturing method and a conventional optical fiber fusion splicer, has strong repeatability, convenient operation and control and low cost, can obtain good transmission spectrum without offset fusion splicing, and is suitable for large-scale production application.
Drawings
FIG. 1 shows an Al-based alloy according to the invention2O3The overall construction of the optical fiber ultraviolet sensor of/ZnO is schematic;
FIG. 2 is a view for further embodying the present invention of a drop single mode fiber, a first fine core fiber, a hollow core fiber, Al2O3The specific schematic diagrams of the/ZnO composite material, the second fine-core optical fiber and the lead-out single-mode optical fiber are shown.
Reference numbers in the figures: 1 light source, 2 leading-in single mode fiber, 3 first thin core fiber, 4 hollow core fiber, 5Al2O3The optical fiber is a composite material of/ZnO, 6 second thin-core optical fibers, 7 leading-out single-mode optical fibers and 8 spectrometers.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings.
FIG. 1 shows an Al-based alloy according to the invention2O3The overall construction of the/ZnO optical fiber ultraviolet sensor is shown schematically. Al-based material constructed according to the invention as shown in FIG. 12O3The optical fiber ultraviolet sensor of/ZnO mainly comprises a light source 1, a lead-in single mode optical fiber 2, a first thin core optical fiber 3, a hollow optical fiber 4 and Al which are connected in sequence2O3The device comprises a/ZnO composite material 5, a second fine-core optical fiber 6, an outgoing single-mode optical fiber 7 and a spectrometer 8. The light source 1 is a broadband light source, has a central wavelength of 1550nm and is used for generating optical signals; introducing a single mode optical fiber 2 for receiving and transmitting light of the light source 1 and transmitting it to a first fine core optical fiber 3; the first thin-core optical fiber 3 is aligned and welded with the leading-in single-mode optical fiber 2, is used for generating interference and coupling the mode of an interference signal to the hollow-core optical fiber 4; the hollow optical fiber 4 is provided with Al therein2O3The two ends of the/ZnO composite material 5 are respectively aligned and welded with the first thin-core optical fiber 3 and the second thin-core optical fiber 6, and an interference signal is output through the leading-out single-mode optical fiber 7; the spectrometer 8 performs transmission spectrum detection on the interference mode output by the leading single-mode fiber 7 and detects the interference mode according to the detectionAnd correspondingly acquiring sensing data by the structure.
Specifically, the optical fiber ultraviolet sensor according to the present invention includes two sections of single mode fibers, i.e., a leading-in single mode fiber 2 and a leading-out single mode fiber 7, and additionally includes two sections of thin core fibers and a section of hollow fiber, i.e., a first thin core fiber 3, a second thin core fiber 6 and a hollow fiber 4. An optical signal sent by a light source 1 enters a first thin core optical fiber 3 through a leading-in single mode optical fiber 2, then enters a hollow optical fiber 4 which is welded with the first thin core optical fiber 3, enters a leading-out single mode optical fiber 7 through a second thin core optical fiber 6, and finally enters a spectrometer 8.
According to a preferred embodiment of the present invention, the length of the first thin-core optical fiber 3 and the second thin-core optical fiber 6 is set to 1.5cm, and the length of the hollow-core optical fiber 4 is set to 2 cm. More tests have shown that the length of the hollow core fiber 4 affects the light energy distribution and determines the coupling strength between the fiber splices.
In order to improve the sensitivity of the sensor to ultraviolet, Al grows in the hollow-core optical fiber 42O3the/ZnO composite material 5 adopts a hydrothermal method with a simple preparation method to grow Al2O3the/ZnO composite material 5. The specific mode is as follows: growing the growth mixed solution in a reaction kettle at 200 ℃ for 20 hours by a hydrothermal method, washing the growth mixed solution by deionized water mostly, freeze-drying the growth mixed solution in vacuum for 24 hours, and calcining the powder of the growth mixed solution at 1200 ℃ for 3 hours to obtain Al2O3Powder, which is used as a raw material and is filled into ZnO solution prepared by a hydrothermal method by 1-5 percent, the cleaned hollow optical fiber (4) is immersed into 1-5 percent of mixed solution prepared by the hydrothermal method for growth for 10 hours at 100 ℃, and then drying treatment is carried out at 60 ℃ to ensure that Al is contained2O3the/ZnO composite material (5) grows in the hollow-core optical fiber (4) to form 350-400nm Al2O3the/ZnO composite material (5).
The measurement principle is as follows:
the light of the light source 1 passes through the leading-in single mode fiber 2, when reaching the fusion point of the leading-in single mode fiber 2 and the first thin core fiber 3, a part of light enters the cladding of the first thin core fiber 3 to excite the cladding mode, a part of light enters the fiber core of the first thin core fiber 3 to excite the fiber core model, and when the light enters the hollow core fiber 4, because the fiber core of the first thin core fiber 3 and the fiber core of the hollow core fiber 4 are not matched, the high-order mode of the hollow core fiber 4 is excited, because of the difference of transmission coefficients, when the light is recoupled to the second thin core fiber 6, the modes can interfere with each other, and the light is received by the spectrometer 8 through the leading-out single mode fiber.
In this embodiment, Al is grown in the hollow-core optical fiber 4 by hydrothermal method2O3the/ZnO composite material 5 is characterized in that when the external ultraviolet environment changes,
the change causes a change in the propagation constant of the hollow-core fiber 4, and thus mode interference phenomenon, that is, an extreme value of the transmission spectrum (the wavelength corresponding to the extreme point is referred to as a characteristic wavelength) shifts, and the change in the characteristic wavelength is represented by Δ λ:
wherein, the lambda is the characteristic wavelength,
for effective index difference, L is the length of the hollow core fiber. The shift of the characteristic wavelength can reflect the change of the external ultraviolet intensity.
The process of fabricating the fiber optic uv sensor according to the present invention will be described in detail below.
Firstly, growing a growth mixed solution in a reaction kettle for 20 hours at 200 ℃ by a hydrothermal method, washing the growth mixed solution by deionized water mostly, freeze-drying the growth mixed solution for 24 hours in vacuum, and calcining powder of the growth mixed solution for 3 hours at 1200 ℃ to obtain Al2O3Powder, which is used as a raw material and is filled into ZnO solution prepared by a hydrothermal method by 1-5 percent, the cleaned hollow optical fiber (4) is immersed into 1-5 percent of mixed solution prepared by the hydrothermal method for growth for 10 hours at 100 ℃, and then drying treatment is carried out at 60 ℃ to ensure that Al is contained2O3the/ZnO composite material (5) grows in the hollow-core optical fiber (4) to form 350-400nm Al2O3a/ZnO composite material (5);
then, preferably adopting a custom mode of an optical fiber fusion splicer commonly used in the market at present, adjusting the discharge intensity to 3500bit, setting the discharge time to 2000ms, fusing the first thin-core optical fiber 3 by aligning the fiber core at one end of the introduced single-mode optical fiber 2, then continuously fusing the hollow-core optical fiber 4 by aligning the fiber core at the other end of the first thin-core optical fiber 3, fusing the second thin-core optical fiber 6 by aligning the fiber core at the other end of the hollow-core optical fiber 4, and finally fusing and leading out the single-mode optical fiber 7 by aligning the fiber core at the other end of the second thin-core optical fiber 6;
and finally, connecting the optical fiber element subjected to the welding with the light source 1 and the spectrometer 8, thereby completing the preparation process of the whole optical fiber ultraviolet sensor.
As can be seen from the above description, the optical fiber ultraviolet sensor according to the present invention can complete the whole manufacturing process only by using a hydrothermal method with a simple manufacturing method and a conventional optical fiber fusion splicer, has strong repeatability, is convenient to operate and control, has low cost, can obtain a good transmission spectrum without offset fusion splicing, can effectively improve the sensitivity of the system, and is suitable for large-scale production.
Claims (6)
1. Based on Al2O3The optical fiber ultraviolet sensor of/ZnO is characterized by comprising a light source (1), a lead-in single mode optical fiber (2), a first thin core optical fiber (3), a hollow core optical fiber (4) and Al which are sequentially connected2O3The optical fiber comprises a/ZnO composite material (5), a second fine-core optical fiber (6), an outgoing single-mode optical fiber (7) and a spectrometer (8), wherein: the light source (1) is a broadband light source, has a central wavelength of 1550nm and is used for generating optical signals; the leading-in single-mode optical fiber (2) is used for receiving and transmitting the light of the light source (1) and transmitting the light to the first thin-core optical fiber (3); the first thin-core optical fiber (3) is aligned and welded with the leading-in single-mode optical fiber (2) and used for generating interference and coupling the mode of an interference signal to the hollow-core optical fiber (4); the hollow-core optical fiber (4) is internally provided with Al2O3a/ZnO composite material (5) having two ends respectively opposed to the first fine core optical fiber (3) and the second fine core optical fiber (6)Quasi-fusion, and outputting the interference signal through leading out a single mode fiber (7); the spectrometer (8) performs transmission spectrum detection on the interference mode output by the leading-out single-mode fiber (7), and correspondingly obtains sensing data according to a detection structure;
the hollow-core optical fiber (4) is internally provided with Al2O3The growth method of the/ZnO composite material (5) comprises the following steps: growing the growth mixed solution in a reaction kettle at 200 ℃ for 20 hours by a hydrothermal method, washing the growth mixed solution for multiple times by deionized water, freeze-drying the growth mixed solution in vacuum for 24 hours, and calcining the powder of the growth mixed solution at 1200 ℃ for 3 hours to obtain Al2O3Powder, which is used as a raw material and is filled into ZnO solution prepared by a hydrothermal method by 1-5 percent, the cleaned hollow optical fiber (4) is immersed into 1-5 percent of mixed solution prepared by the hydrothermal method for growth for 10 hours at 100 ℃, and then drying treatment is carried out at 60 ℃ to ensure that Al is contained2O3the/ZnO composite material (5) grows in the hollow-core optical fiber (4) to form 350-400nm Al2O3the/ZnO composite material (5).
2. The fiber optic uv sensor according to claim 1, characterized in that the first and second fine-core optical fibers (3, 6) are set to 1.5cm in length.
3. The fiber optic uv sensor according to claim 1, characterized in that Al is grown in the hollow-core fiber (4)2O3The length of the/ZnO composite material (5) was set to 2 cm.
4. Based on Al for manufacturing2O3Method for a/ZnO fibre optic uv sensor, characterized in that the method comprises the steps of: growing the growth mixed solution in a reaction kettle at 200 ℃ for 20 hours by a hydrothermal method, washing the growth mixed solution for multiple times by deionized water, freeze-drying the growth mixed solution in vacuum for 24 hours, and calcining the powder of the growth mixed solution at 1200 ℃ for 3 hours to obtain Al2O3Powder, which is used as a raw material and is filled into ZnO solution prepared by a hydrothermal method by 1 to 5 percent, and the cleaned hollow-core optical fiber (4) is immersed into 1 to 5 percent of mixed solution prepared by the hydrothermal method for growth at 100 DEG CAfter 10 hours, Al was allowed to stand by drying at 60 ℃ to2O3the/ZnO composite material (5) grows in the hollow-core optical fiber (4) to form 350-400nm Al2O3a/ZnO composite material (5); the method comprises the steps that a user-defined mode of an optical fiber fusion splicer is adopted, the discharge intensity is adjusted to be 3500bit, the discharge time is 2000ms, one end of a single-mode fiber (2) is led in to be fused with a first thin-core fiber (3) in a fiber core alignment mode, then a hollow-core fiber (4) is continuously fused at the other end of the first thin-core fiber (3) in a fiber core alignment mode, then a second thin-core fiber (6) is fused at the other end of the hollow-core fiber (4) in a fiber core alignment mode, and finally a single-mode fiber (7) is led out in a fiber core alignment mode at the other end of the second thin-; and connecting the optical fiber element subjected to the welding with a light source (1) and a spectrometer (8), thereby completing the preparation process of the whole optical fiber ultraviolet sensor.
5. A method for making Al-based alloy according to claim 42O3Method for a/ZnO fibre optic uv sensor, characterized in that in step (1) the length of the hollow core fibre (4) is set to 2 cm.
6. A method for making Al-based alloy according to claim 42O3Method of fiber optic uv sensor/ZnO characterized in that in step (2) the first fine core fiber (3) and the second fine core fiber (6) length is set to 1.5 cm.
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