CN109655159A - Based on Al2O3Optical fiber Ultraviolet sensor of/ZnO and preparation method thereof - Google Patents

Based on Al2O3Optical fiber Ultraviolet sensor of/ZnO and preparation method thereof Download PDF

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CN109655159A
CN109655159A CN201910051612.6A CN201910051612A CN109655159A CN 109655159 A CN109655159 A CN 109655159A CN 201910051612 A CN201910051612 A CN 201910051612A CN 109655159 A CN109655159 A CN 109655159A
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optical fiber
fiber
core
hollow
thin
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沈涛
代小爽
冯月
李晓晓
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Harbin Qingcen Technology Co ltd
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Harbin University of Science and Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28Investigating the spectrum
    • G01J3/45Interferometric spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02Details

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  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
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Abstract

The invention discloses be based on Al2O3The optical fiber Ultraviolet sensor of/ZnO, including sequentially connected light source, introducing single mode optical fiber, the first thin-core fibers, hollow-core fiber, Al2O3/ ZnO, the second thin-core fibers draw single mode optical fiber and spectrometer, and light source is wideband light source, central wavelength 1550nm;Introducing single mode optical fiber is used to receive and the light of transmission light source, and is transmitted to the first thin-core fibers;It first thin-core fibers and introduces single mode optical fiber and aligns welding, generate interference, and by interference signal Mode Coupling to hollow-core fiber;Al is set inside hollow-core fiber2O3/ ZnO, both ends align welding in the first thin-core fibers and the second thin-core fibers, and interference signal is drawn single mode optical fiber output;Spectrometer executes spectral detection to the interference pattern for drawing single mode optical fiber, and obtains sensing data.The invention also discloses corresponding production methods.According to the present invention by means of Al2O3/ ZnO enhancing significantly improves system sensitivity to ultraviolet absorbability, obtains and makes simply, convenient for the optical fiber Ultraviolet sensor of encapsulation.

Description

Based on Al2O3Optical fiber ultraviolet sensor of/ZnO and manufacturing method thereof
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 UV fiber sensors, and in the prior art, Azad et al ("Azad S, Parvizi R, Sadeghi E. Side-detecting optical fiber coated with Zn (OH)2nanorods for ultraviolet sensing applications, LaserPhysics, 2017, 27(9): 095901.) reported Zn (OH) -based2The nanorod fiber ultraviolet sensor is characterized in that Zn (OH) grows on the multimode micro-nano fiber by a chemical corrosion method2The nano rod has certain potential safety hazard in the process of manufacturing the micro-nano optical fiber, and can correspondingly cause the problems of low success rate, difficult packaging and the like of an optical 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 DEG CFiring 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 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, 5 Al2O3The 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 ZnO optical fiber ultraviolet sensor mainly comprises a plurality of optical fiber ultraviolet sensors which are connected in sequenceLight source 1, leading-in single mode fiber 2, first thin-core fiber 3, hollow-core fiber 4 and Al2O3The 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-out single-mode fiber 7, and correspondingly obtains sensing data according to the detection 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 mixed solution by hydrothermal methodAfter growing for 20 hours at 200 ℃ in a reaction kettle, mostly washing by deionized water, freeze-drying for 24 hours in vacuum, and calcining the powder 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 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 used when the external ultraviolet environment changesThe change causes a change in the propagation constant of the hollow-core optical fiber 4, and thus mode interference phenomenon, in which the extreme value of the transmission spectrum (the wavelength corresponding to the extreme point is referred to as the characteristic wavelength) shifts, occurs, and the change in the characteristic wavelength is expressed as
Wherein,in order to be a characteristic wavelength of the light,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 (7)

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 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.
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. The fiber optic uv sensor according to claim 1, characterized in that Al is grown inside the hollow-core 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 air350-400nm Al is formed inside the core fiber (4)2O3the/ZnO composite material (5).
5. 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 1-5 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);
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.
6. The method according to claim 5, wherein in step (1), the length of the hollow-core optical fiber (4) is set to 2 cm.
7. The method according to claim 5, wherein 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.
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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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