CN112731585B - Method for preparing sapphire regenerated grating high-temperature sensor by utilizing high-temperature annealing - Google Patents
Method for preparing sapphire regenerated grating high-temperature sensor by utilizing high-temperature annealing Download PDFInfo
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- CN112731585B CN112731585B CN202011442905.6A CN202011442905A CN112731585B CN 112731585 B CN112731585 B CN 112731585B CN 202011442905 A CN202011442905 A CN 202011442905A CN 112731585 B CN112731585 B CN 112731585B
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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
- G02B6/02123—Refractive index modulation gratings, e.g. Bragg gratings characterised by the method of manufacture of the grating
- G02B6/02133—Refractive index modulation gratings, e.g. Bragg gratings characterised by the method of manufacture of the grating using beam interference
- G02B6/02138—Refractive index modulation gratings, e.g. Bragg gratings characterised by the method of manufacture of the grating using beam interference based on illuminating a phase mask
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
- G01K11/32—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using changes in transmittance, scattering or luminescence in optical fibres
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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
- G02B6/02123—Refractive index modulation gratings, e.g. Bragg gratings characterised by the method of manufacture of the grating
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- Engineering & Computer Science (AREA)
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- Optics & Photonics (AREA)
- Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)
- Measuring Temperature Or Quantity Of Heat (AREA)
Abstract
The invention provides a method for manufacturing a sapphire high-temperature sensor of a regenerated grating by firstly etching an original grating by femtosecond laser and then manufacturing the regenerated grating by a high-temperature annealing mode. Exposing a Bragg grating on a sapphire optical fiber by femtosecond laser through a phase mask, gradually raising the temperature to 1100 ℃ after placing the initial grating in a high-temperature furnace with the initial temperature of 100 ℃, and annealing the optical fiber to 30 ℃ after placing the optical fiber at the high temperature of 1100 ℃ for 10min to generate the high-temperature grating. The sapphire sensor manufactured by the method has more stable high-temperature measurement performance and has important significance on a measurement system with high requirement on high-temperature performance.
Description
Technical Field
The invention belongs to the field of optical fiber sensing, and particularly relates to a method for preparing a sapphire regenerated grating high-temperature sensor by using high-temperature annealing.
Background
In the measurement for ultra-high temperature, the temperature resistance of a common sensor is poor, and the sensitivity is poor in a complex and ultra-high temperature environment, so that the measurement of ultra-high temperature by aerospace and oil wells, for example, is influenced and restricted. High temperature sensors made of sapphire fibers have been produced and are regarded by people. Compared with the traditional optical fiber device, the sapphire optical fiber is largely used in the optical fiber measurement field because of the inherent characteristics of the sapphire optical fiber, such as high melting point and high transmission efficiency of infrared band signals. However, the conventional engraved fiber bragg grating is easily erased at high temperature, and loses its high temperature measurement effect, so that a method for manufacturing a stable regenerated grating high-temperature sensor by using femtosecond laser to firstly manufacture an original bragg grating by using a phase mask in a sapphire fiber and then using high-temperature annealing is proposed, and the high-temperature performance of the regenerated grating is about 1500 ℃.
The fiber grating is mainly classified into a reflection type grating period (Λ <1 μm) and a long period (Λ >1 μm). The grating satisfying the Bragg equation lambda =2neff lambda is called Bragg grating, and the writing mode of the uniform Bragg grating mainly comprises femtosecond laser phase mask writing and direct writing. The grating is easy to erase at high temperature by using a phase mask plate writing mode, and the regenerated grating can effectively enhance the high-temperature performance of the grating, so that the grating engraved by an exposure method cannot be erased at high temperature.
The fiber grating makes optical signals particularly sensitive to external high temperature by using thermal expansion and thermo-optic effect, and the sapphire sensor prepared by the method is very sensitive, has good repeated processing performance, and can be produced and processed in large scale to a certain extent.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for preparing a sapphire regenerated grating high-temperature sensor by high-temperature annealing.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a method for preparing a sapphire regenerated grating high-temperature sensor by using high-temperature annealing comprises the following steps: step a, sequentially putting the sapphire optical fiber into 36% concentrated hydrochloric acid, acetone and alcohol, respectively cleaning for 10 minutes, drying for 10 minutes after cleaning, and carrying out chemical mechanical polishing on the dried sapphire optical fiber; b, performing ultrasonic cleaning on the polished sapphire optical fiber, and placing the cleaned sapphire optical fiber under a laser writing phase mask plate for writing to form a sapphire optical fiber original grating; c, annealing the sapphire optical fiber original grating at high temperature: heating the sapphire optical fiber original grating to 850 ℃ within one hour, keeping the temperature for 50 minutes, and then slowly reducing the temperature to 300 ℃ within another hour to generate a regenerated grating; d, performing post annealing on the regenerated grating for stabilizing treatment: and controlling the temperature of the regenerated grating to rise to 1100 ℃ within 20 minutes and keeping the temperature for 20 minutes to obtain the sapphire optical fiber regenerated grating sensor.
Preferably, when the sapphire optical fiber is subjected to chemical mechanical polishing operation in the step a, the rotation speed of the polishing head and the polishing pad is 70r/min, the polishing pressure polishing solution is silicon dioxide polishing solution, the flow rate of the polishing solution is 90ml/min, and the polishing pressure is 49kpa.
Preferably, the post annealing mode is adopted in the step d, and the reflectivity of the sapphire optical fiber regeneration grating sensor is 0.15db.
A sapphire fiber regeneration grating high-temperature measurement method comprises the following steps: the method comprises the following steps that (1) a sapphire optical fiber regeneration grating sensor is placed in a high-temperature furnace, and three interfaces of a circulator are sequentially connected with a broadband light source, a spectrometer and the sapphire optical fiber regeneration grating sensor; and (2) adjusting the temperature of the high-temperature furnace during measurement, transmitting light to the fiber grating end of the sapphire fiber regeneration grating sensor through the circulator by the broadband light source, reflecting the light with a specific wavelength to the spectrometer through the circulator by the fiber grating end, and analyzing by the spectrometer.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention uses the sapphire optical fiber, and has good performance at high temperature;
2. the grating is manufactured by using a regeneration grating mode, the performance of the grating is not easy to erase at high temperature, and the performance of the sensor is excellent.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
Drawings
Further objects, features and advantages of the present invention will become apparent from the following description of embodiments of the invention, with reference to the accompanying drawings, in which:
FIG. 1 schematically illustrates a femtosecond laser phase mask writing schematic diagram according to the present invention;
FIG. 2 is a schematic diagram of the original grating of the sapphire fiber of the present invention;
FIG. 3 is a schematic diagram of a sapphire fiber-regenerating grating pyrometry method of the present invention;
FIG. 4 is a graph schematically showing the relationship between the central wavelength and the temperature of the sapphire fiber regeneration grating of the present invention.
In the figure:
1. cylindrical lens 2, phase mask
3. Sapphire optical fiber 4, sapphire optical fiber original grating
5. Broadband light source 6 and spectrometer
7. Circulator 8 and high-temperature furnace
9. Sapphire optical fiber regeneration grating sensor
Detailed Description
The objects and functions of the present invention and methods for accomplishing the same will be apparent by reference to the exemplary embodiments. However, the present invention is not limited to the exemplary embodiments disclosed below; it can be implemented in different forms. The nature of the description is merely to assist those skilled in the relevant art in a comprehensive understanding of the specific details of the invention.
Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings. In the drawings, the same reference numerals denote the same or similar parts, or the same or similar steps.
The high temperature sensor for sapphire regenerated grating is prepared by femtosecond laser and high temperature annealing method, and belongs to the field of optical fiber sensing.
In order to achieve the above-listed purposes, the technical scheme adopted by the invention is as follows: the femtosecond laser used in the invention is produced by coherent company, the central wavelength is 800nm, the pulse width is 50fs, and the repetition frequency is 1000hz. The original grating first made using the phase mask is written as shown in figure 1.
Firstly, cutting a sapphire optical fiber according to a required length, sequentially putting the single crystal optical fiber into 36% concentrated hydrochloric acid, acetone and alcohol for cleaning for ten minutes, drying for 10 minutes after cleaning, and performing chemical mechanical polishing, wherein a polishing head in a polishing method is in contact with a polishing pad and polishing liquid under certain pressure and rotates in the same direction with the polishing pad, the rotating speed of the polishing head and the polishing pad in the experiment is 70r/min, the polishing pressure polishing liquid adopts silicon dioxide polishing liquid, the flow speed of the polishing liquid is 90ml/min, the polishing pressure is 49kpa, finally, the chemical mechanical polishing of sapphire is realized, and the polished sapphire optical fiber is subjected to ultrasonic cleaning. And finally, placing the cleaned sapphire optical fiber under a laser writing phase mask plate for preparing for writing. The schematic of the exposed grating is shown in figure 2.
Then, carrying out high-temperature annealing on the original grating: the temperature was raised to 850 ℃ for 1 hour and held for 50 minutes, after which it was slowly lowered to 300 ℃ for another 1 hour, and a regenerated grating appeared (the original grating was erased). And then stabilizing the regenerated grating, and raising the temperature to 1100 ℃ within 20 minutes and keeping the temperature for 20 minutes after the regenerated grating is saturated by adopting a post-annealing mode. The regeneration grating is formed at 800 ℃, the temperature is continuously raised to 1100 ℃, and the reflectivity of the grating can be maintained at 0.15db through a post-annealing mode.
The sapphire fiber grating pyrometry method is shown in fig. 3. The sapphire optical fiber regeneration grating sensor is arranged in a high-temperature furnace 8 and is connected with a broadband light source 5 and a spectrometer 6 through a circulator 7, an optical fiber sensing analyzer produced by Yokogawa company is adopted as analysis equipment of the spectrometer 6, the reflection spectrum of the sensor is measured in the experiment, the broadband light source 5 transmits light to an optical fiber grating end of the sapphire optical fiber regeneration grating sensor 9, and the grating reflects the light with specific wavelength back and transmits the light into the spectrometer 6 for analysis. The sapphire fiber regeneration grating sensor 9 is placed in a high-temperature furnace 8, and the temperature is calibrated by using the change of the wavelength.
The sapphire fiber-optic regeneration grating sensor 9 first measures the waveform thereof in the high-temperature furnace 8 in an unheated state. And then heating the fiber grating to 50 ℃ in sequence, recording the reflection spectrum waveform of the fiber grating in sequence every 50 ℃, and obtaining the central wavelength of the fiber grating. And a graph of its center wavelength versus temperature is plotted as shown in fig. 4.
The invention has the beneficial effects that: the invention uses the sapphire optical fiber, and has good performance at high temperature; the grating is manufactured by using a regeneration grating mode, the performance of the grating is not easy to erase at high temperature, and the performance of the sensor is excellent.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
Claims (2)
1. A method for preparing a sapphire regeneration grating high-temperature sensor by using high-temperature annealing is characterized by comprising the following steps:
step a, sequentially putting the sapphire optical fiber into 36% concentrated hydrochloric acid, acetone and alcohol, respectively cleaning for 10 minutes, drying for 10 minutes after cleaning, and carrying out chemical mechanical polishing on the dried sapphire optical fiber;
b, performing ultrasonic cleaning on the polished sapphire optical fiber, and placing the cleaned sapphire optical fiber under a laser writing phase mask plate for writing to form a sapphire optical fiber original grating;
c, annealing the sapphire optical fiber original grating at high temperature: heating the sapphire optical fiber original grating to 850 ℃ within one hour, keeping the temperature for 50 minutes, and then slowly reducing the temperature to 300 ℃ within another hour to generate a regenerated grating;
d, performing post annealing on the regenerated grating for stabilizing treatment: controlling the temperature of the regenerated grating to rise to 1100 ℃ within 20 minutes and keeping for 20 minutes to obtain a sapphire fiber regenerated grating sensor;
the reflectivity of the sapphire fiber regeneration grating sensor is 0.15db.
2. The method as claimed in claim 1, wherein the sapphire optical fiber is subjected to chemical mechanical polishing in step a, the rotation speed of the polishing head and the polishing pad is 70r/min, the polishing pressure is silica polishing solution, the flow rate of the polishing solution is 90ml/min, and the polishing pressure is 49kpa.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102053105A (en) * | 2010-11-23 | 2011-05-11 | 吉林大学 | Method for detecting thermal effect of interaction of laser and matter by using fiber grating |
| WO2013051614A1 (en) * | 2011-10-07 | 2013-04-11 | 株式会社豊田自動織機 | Method for manufacturing optical fiber for sensor, and optical fiber for sensor |
| CN103674085A (en) * | 2013-12-16 | 2014-03-26 | 西安电子科技大学 | U-shaped structure sapphire fiber grating temperature and stress sensor and manufacturing method thereof |
| CN107014520A (en) * | 2017-05-18 | 2017-08-04 | 中国航空工业集团公司北京长城计量测试技术研究所 | A kind of capillary type high temperature fiber grating temperature sensor and preparation method thereof |
| CN108106751A (en) * | 2017-12-13 | 2018-06-01 | 俞婷 | The preparation process of sapphire photonic crystal fiber grating superhigh temperature distributed sensor |
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2020
- 2020-12-08 CN CN202011442905.6A patent/CN112731585B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102053105A (en) * | 2010-11-23 | 2011-05-11 | 吉林大学 | Method for detecting thermal effect of interaction of laser and matter by using fiber grating |
| WO2013051614A1 (en) * | 2011-10-07 | 2013-04-11 | 株式会社豊田自動織機 | Method for manufacturing optical fiber for sensor, and optical fiber for sensor |
| CN103674085A (en) * | 2013-12-16 | 2014-03-26 | 西安电子科技大学 | U-shaped structure sapphire fiber grating temperature and stress sensor and manufacturing method thereof |
| CN107014520A (en) * | 2017-05-18 | 2017-08-04 | 中国航空工业集团公司北京长城计量测试技术研究所 | A kind of capillary type high temperature fiber grating temperature sensor and preparation method thereof |
| CN108106751A (en) * | 2017-12-13 | 2018-06-01 | 俞婷 | The preparation process of sapphire photonic crystal fiber grating superhigh temperature distributed sensor |
Non-Patent Citations (1)
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| 高温退火制备再生光纤光栅的光谱重复性;王涛 等;《光谱学与光谱分析》;20130531;第33卷(第05期);第1411-1414页 * |
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