CN116448681A - Hydrogen sensor probe utilizing reference fiber bragg grating and preparation method thereof - Google Patents

Hydrogen sensor probe utilizing reference fiber bragg grating and preparation method thereof Download PDF

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CN116448681A
CN116448681A CN202310358379.2A CN202310358379A CN116448681A CN 116448681 A CN116448681 A CN 116448681A CN 202310358379 A CN202310358379 A CN 202310358379A CN 116448681 A CN116448681 A CN 116448681A
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fiber
bragg grating
optical fiber
test
hydrogen sensor
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陈均
陈昱霖
袁登鹏
姚运喜
杨轶飞
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Institute of Materials of CAEP
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation

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Abstract

The invention discloses a hydrogen sensor probe using a reference fiber bragg grating and a preparation method thereof, relating to the field of fiber hydrogen sensors, comprising the following steps: the optical fiber testing device comprises a testing optical fiber and a reference optical fiber, wherein a Bragg grating area is arranged in each of the testing optical fiber and the reference optical fiber, and a cladding of the Bragg grating area is thinned after corrosion; uniformly coating the periphery of a Bragg grating area in the test optical fiber; the test optical fiber and the reference optical fiber are sealed into a whole, and are coupled and connected together through an optical fiber coupling branching device; the fiber bragg grating demodulator demodulates and analyzes the spectrum signals after being coupled by the fiber bragg grating coupling branching device; according to the invention, the influence of temperature fluctuation on the test can be eliminated by using the packaging mode of the reference fiber grating, and the accuracy of the hydrogen sensor probe is improved.

Description

Hydrogen sensor probe utilizing reference fiber bragg grating and preparation method thereof
Technical Field
The invention relates to the field of optical fiber hydrogen sensors, in particular to a hydrogen sensor probe utilizing a reference fiber bragg grating and a preparation method thereof.
Background
The statements in this section merely provide background information related to the present disclosure and may not constitute prior art.
Hydrogen monitoring is a key technology for realizing safe production, and has important application in the fields of hydrogen energy and national defense; the hydrogen sensor has the characteristics of small size and portability, is suitable for hydrogen monitoring in different scenes, and is the current research focus for developing a novel hydrogen sensor; the optical fiber type hydrogen sensor uses light as a transmission medium, has the advantages of intrinsic safety, electromagnetic interference resistance and use in toxic environments, and is a sensor with wide application prospect; how to improve the testing accuracy and long-term stability of the sensor is a current difficult problem, and the current research is mainly started from the aspects of optical fiber sensing principle, hydrogen sensitive material, probe structure and the like; the probe structure can be optimized for all sensors, has universality and is a key technology for improving the performance of the sensors; chinese patent CN205404392U writes two spaced Bragg gratings (FBGs) on the same optical fiber, one grating is used for temperature compensation and one grating is used for hydrogen sensing, so that the temperature compensated hydrogen sensor is realized, and the accuracy of probe testing of hydrogen concentration is improved; chinese patent CN107607218B sets up two FBGs on same optic fibre, and one FBG regional gilt membrane and PTFE film, one FBG regional plating polydopamine membrane, hydrogen sensitive membrane and PTFE film have realized measuring temperature and hydrogen concentration simultaneously, have eliminated the influence of temperature to hydrogen concentration.
The fiber sensor commonly used at present mainly sets a plurality of FBG areas on the same optical fiber, and simultaneously realizes measurement of various parameters such as temperature, hydrogen and the like; on the basis, the influence of temperature fluctuation on the hydrogen concentration test can be eliminated through the temperature test; however, the disadvantage of providing multiple FBGs on the same fiber is that: 1. the FBGs are spaced, and different FBGs do not measure the same space region, so that the compensation effect is greatly reduced in an environment with uneven steps at certain temperatures and hydrogen concentration; 2. the same optical fiber is provided with a plurality of FBG areas, so that the complexity of coating films of different FBG areas can be increased, and the operation difficulty is increased in the actual coating process.
Disclosure of Invention
The invention aims at: aiming at the problems in the prior art, the hydrogen sensor probe utilizing the reference fiber grating and the preparation method thereof are provided, the response to the temperature of a test environment is realized by utilizing the reference fiber, the accuracy of hydrogen measurement is improved, the reference fiber grating and the test fiber grating are separated, and the flexibility of surface coating of the reference fiber grating and the test fiber grating is improved, so that the problems are solved.
The technical scheme of the invention is as follows:
a hydrogen sensor probe utilizing a reference fiber bragg grating, comprising:
the optical fiber testing device comprises a testing optical fiber and a reference optical fiber, wherein a Bragg grating area is arranged in each of the testing optical fiber and the reference optical fiber, and a cladding of the Bragg grating area is thinned after corrosion; uniformly coating the periphery of a Bragg grating area in the test optical fiber;
the test optical fiber and the reference optical fiber are sealed into a whole, and are coupled and connected together through an optical fiber coupling branching device;
and the fiber bragg grating demodulator demodulates and analyzes the spectrum signals after being coupled by the fiber bragg grating coupling branching device.
Further, the cladding of the Bragg grating areas of the test optical fiber and the reference optical fiber is thinned through hydrofluoric acid corrosion so as to improve the sensitivity of the optical fiber to strain.
Further, the test optical fiber and the reference optical fiber both adopt single-mode optical fiber gratings;
the cladding outside diameter of the non-corroded area of the test optical fiber and the reference optical fiber is 125 mu m, the diameter of the fiber core of the optical fiber is 8-10 mu m, the length of the Bragg grating area is 10mm, the reflection center wavelength of the optical fiber grating is 1510-1590 nm, the reflectivity is more than 90%, the 3dB bandwidth is 0.22nm, and the side mode suppression ratio is 18-22dB.
Further, the cladding of the Bragg grating areas of the test optical fiber and the reference optical fiber has an outer diameter of 20-50 μm after being corroded by hydrofluoric acid.
Further, the periphery of the Bragg grating area in the test optical fiber is sequentially plated with a Ti film, a PdAG alloy film and a Pd film.
Further, the thickness of the Ti film is 5-10nm;
the thickness of the PdAG alloy film is 50-500nm;
the thickness of the Pd film is 5-20nm.
Further, the test optical fiber and the reference optical fiber are packaged into a stainless steel sleeve, and the tail is sealed by epoxy resin glue.
A method for preparing a hydrogen sensor probe by using a reference fiber bragg grating comprises the following steps:
step S1: preprocessing two single-mode fiber gratings;
step S2: taking the pretreated single-mode fiber gratings as a substrate, and uniformly coating the periphery of a Bragg grating area of one single-mode fiber grating;
step S3: taking a coated single-mode fiber grating as a test fiber, taking an uncoated single-mode fiber grating as a reference fiber, sealing the test fiber and the reference fiber into a whole, and coupling and connecting the test fiber and the reference fiber together through a fiber coupling branching device;
step S4: and demodulating and analyzing the spectrum signals after being coupled by the fiber coupling branching device through the fiber grating demodulator.
Further, a Bragg grating area is arranged in the single-mode fiber grating;
the preprocessing in step S1 includes:
corroding and thinning the cladding of the Bragg grating area by adopting hydrofluoric acid;
the plating film in the step S2 includes:
uniformly plating Ti films, pdAG alloy films and Pd films on the periphery of the Bragg grating area in sequence by adopting a magnetron sputtering mode;
the step S3 includes:
packaging the test optical fiber and the reference optical fiber into a stainless steel sleeve, and sealing the tail part by adopting epoxy resin glue;
the test optical fiber and the reference optical fiber are connected to the optical fiber coupling branching device, and the optical fiber coupled by the optical fiber coupling branching device is connected to the optical fiber grating demodulator.
Further, the cladding of the single-mode fiber grating has an outer diameter of 125 mu m, the fiber core has a diameter of 8-10 mu m, the length of the Bragg grating area is 10mm, the reflection center wavelength of the single-mode fiber grating is 1510-1590 nm, the reflectivity is more than 90%, the 3dB bandwidth is 0.22nm, and the side mode suppression ratio is 18-22dB;
the outer diameter of the cladding of the Bragg grating area is 20-50 mu m after being corroded by hydrofluoric acid;
the thickness of the Ti film is 5-10nm, the thickness of the PdAG alloy film is 50-500nm, and the thickness of the Pd film is 5-20nm.
Compared with the prior art, the invention has the beneficial effects that:
1. the hydrogen sensor probe using the reference fiber bragg grating and the preparation method thereof can eliminate the influence of temperature fluctuation on the test and improve the accuracy of the hydrogen sensor probe by using the packaging mode of the reference fiber bragg grating.
2. The hydrogen sensor probe utilizing the reference fiber bragg grating and the preparation method thereof belong to two optical fibers, the flexibility of probe preparation is improved, the reference fiber bragg grating and the test fiber bragg grating are almost positioned at the same position in space during packaging, and measurement errors caused by space position deviation can be avoided.
Drawings
FIG. 1 is a schematic diagram of a test fiber in a hydrogen sensor probe using a reference fiber grating;
FIG. 2 is a schematic diagram of a hydrogen sensor probe test using a reference fiber grating.
Reference numerals: 1-test optical fiber, 2-reference optical fiber, 3-Bragg grating area, 4-optical fiber core, 5-film, 6-stainless steel sleeve, 7-optical fiber coupling branching device and 8-optical fiber grating demodulation instrument.
Detailed Description
It is noted that relational terms such as "first" and "second", and the like, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The features and capabilities of the present invention are described in further detail below in connection with examples.
Example 1
It should be noted that, in order to facilitate understanding of the technical solution of the present invention, the following terms are explained.
Fiber bragg gratings: the grating with periodically distributed spatial phase is formed in the fiber core, and can form a narrow-band filter or reflector for light in the fiber core, thus being used for manufacturing various fiber devices with unique performance.
Fiber Bragg grating hydrogen sensor: the hydrogen sensor is prepared by utilizing the fiber bragg grating, and the principle is that a hydrogen sensitive film material is deposited around a fiber bragg grating area by utilizing the reflection characteristic of the fiber bragg grating to light, and the change of the reflection center wavelength of the fiber bragg grating is realized by the stress change caused by the action of hydrogen and the film, so that the hydrogen is sensed.
The invention mainly solves the problem that the test signal of the fiber Bragg grating hydrogen sensor is influenced by environmental factors; the reflection center wavelength of the fiber Bragg grating changes along with temperature and strain; when the optical fiber is used as a hydrogen sensor, the metal film plated on the side surface of the optical fiber absorbs hydrogen to cause the axial strain of the optical fiber, so that the change of the reflection center wavelength is caused; in the actual test, the temperature of the environment fluctuates, and other accidental factors such as vibration and the like can exist in the environment; how to eliminate the influence of environmental factors in the design and preparation of the probe and improve the stability of the probe test is a key technology for realizing the wide application of the fiber Bragg grating hydrogen sensor.
Referring to fig. 1-2, this embodiment provides a hydrogen sensor probe using a reference fiber bragg grating, including:
the optical fiber testing device comprises a testing optical fiber 1 and a reference optical fiber 2, wherein a Bragg grating region 3 is arranged in each of the testing optical fiber 1 and the reference optical fiber 2 (namely, only one Bragg grating region 3 is arranged in each of the testing optical fiber 1 and the reference optical fiber 2, and the Bragg grating region 3 is also called as an FBG region), and a cladding of the Bragg grating region 3 becomes thinner after being corroded; the periphery of the Bragg grating area 3 in the test optical fiber 1 is uniformly coated with a film 5, namely the periphery of the Bragg grating area 3 in the test optical fiber 1 is uniformly coated with the film; the cladding of the optical fiber is thinned through corrosion, so that the sensitivity of the optical fiber to strain is improved, and the sensitivity of the hydrogen sensor is improved;
the test optical fiber 1 and the reference optical fiber 2 are sealed into a whole, and the test optical fiber 1 and the reference optical fiber 2 are coupled and connected together through an optical fiber coupling branching device 7; namely, taking the optical fiber with the plated film 5 as a test optical fiber 1, taking the optical fiber which is not plated with the corrosion pretreatment as a reference optical fiber 2, and packaging the test optical fiber 1 and the reference optical fiber 2 together;
the fiber bragg grating demodulator 8 is used for demodulating and analyzing the spectrum signals after being coupled by the fiber bragg grating demodulator 8 and the fiber bragg coupling branching device 7; i.e. the fiber grating demodulator 8 collects the sum of the reflected center wavelengths of the test fiber 1 and the reference fiber 2 at the same time.
In this embodiment, specifically, the cladding layers of the bragg grating regions 3 of the test optical fiber 1 and the reference optical fiber 2 are thinned by etching with hydrofluoric acid to improve the sensitivity of the optical fiber to strain; preferably, hydrofluoric acid with a concentration of 10% -40% is used for etching.
In this embodiment, specifically, the test optical fiber 1 and the reference optical fiber 2 both use single-mode fiber gratings;
the cladding outside diameter of the non-corroded area of the test optical fiber 1 and the reference optical fiber 2 is 125 mu m, the diameter of the optical fiber core 4 is 8-10 mu m, the length of the Bragg grating area 3 is 10mm, the reflection center wavelength of the fiber grating is 1510-1590 nm, the reflectivity is >90%, the 3dB bandwidth is 0.22nm, and the side mode suppression ratio is 18-22dB.
In this embodiment, specifically, the cladding layers of the bragg grating regions 3 of the test optical fiber 1 and the reference optical fiber 2 have an outer diameter of 20-50 μm after being etched by hydrofluoric acid.
In this embodiment, specifically, the periphery of the bragg grating region 3 in the test optical fiber 1 is sequentially plated with a Ti film, a PdAg alloy film and a Pd film.
In this embodiment, specifically, the thickness of the Ti film is 5-10nm;
the thickness of the PdAG alloy film is 50-500nm;
the thickness of the Pd film is 5-20nm.
In this embodiment, specifically, the test optical fiber 1 and the reference optical fiber 2 are encapsulated into a stainless steel sleeve 6, and the tail is sealed by epoxy resin glue; preferably, the test fiber 1 and the reference fiber 2 are encapsulated in a stainless steel sleeve 6 of 3mm diameter.
The embodiment also provides a preparation method of the hydrogen sensor probe by using the reference fiber bragg grating, which comprises the following steps:
step S1: preprocessing two single-mode fiber gratings;
step (a) S2: taking the pretreated single-mode fiber gratings as a substrate, and uniformly coating the periphery of a Bragg grating area 3 of one single-mode fiber grating;
step S3: taking a coated single-mode fiber grating as a test optical fiber 1, taking an uncoated single-mode fiber grating as a reference optical fiber 2, sealing the test optical fiber 1 and the reference optical fiber 2 into a whole, and coupling and connecting the test optical fiber 1 and the reference optical fiber 2 together through an optical fiber coupling branching device 7;
step S4: the spectral signal coupled by the fiber coupling splitter 7 is demodulated and analyzed by the fiber grating demodulator 8.
In this embodiment, specifically, a bragg grating region 3 is disposed inside the single-mode fiber grating;
the preprocessing in step S1 includes:
corroding and thinning the cladding of the Bragg grating area 3 by adopting hydrofluoric acid; preferably, the concentration of hydrofluoric acid is 10% -40%;
the plating film in the step S2 includes:
uniformly plating Ti films, pdAG alloy films and Pd films on the periphery of the Bragg grating area 3 in sequence by adopting a magnetron sputtering mode;
the step S3 includes:
packaging the test optical fiber 1 and the reference optical fiber 2 into a stainless steel sleeve 6, and sealing the tail part by adopting epoxy resin glue;
the test optical fiber 1 and the reference optical fiber 2 are connected to the optical fiber coupling branch 7, and the optical fiber coupled by the optical fiber coupling branch 7 is connected to the optical fiber grating demodulator 8.
In this embodiment, specifically, the cladding outer diameter of the single-mode fiber grating is 125 μm, the diameter of the fiber core 4 is 8-10 μm, the length of the bragg grating region 3 is 10mm, the reflection center wavelength of the single-mode fiber grating is 1510-1590 nm, the reflectivity is >90%, the 3dB bandwidth is 0.22nm, and the side mode suppression ratio is 18-22dB;
the outer diameter of the cladding of the Bragg grating area 3 is 20-50 mu m after being corroded by hydrofluoric acid;
the thickness of the Ti film is 5-10nm, the thickness of the PdAG alloy film is 50-500nm, and the thickness of the Pd film is 5-20nm.
The data processing details of the hydrogen sensor probe based on the reference fiber bragg grating are as follows:
the reflection center wavelength of the reference fiber varies with temperature, and the amount of wavelength variation with temperature can be given by equation 1:
Δλ 1 =λ 1 (α+ξ)ΔT (1)
wherein:
λ 1 representing the reflected center wavelength of the reference fiber;
Δλ 1 representing the reflection center wavelength variation of the reference fiber;
alpha represents the thermo-optic coefficient of the reference fiber;
ζ represents the elasto-optical coefficient of the reference fiber;
Δt represents the amount of temperature change.
The reflection center wavelength of the test fiber changes with temperature and hydrogen concentration, and the wavelength change amount thereof with temperature change can be given by formula 2:
wherein:
λ 2 representing the reflected center wavelength of the test fiber;
Δλ 2 representing the reflection center wavelength variation of the test fiber;
p represents hydrogen partial pressure (hydrogen concentration);
k represents Sievert constant of film hydrogen absorption;
a and b respectively represent the diameters of the optical fiber before and after film coating;
Y F and Y Pd Young's modulus of the test optical fiber and Pd alloy film are respectively shown;
alpha represents the thermo-optic coefficient of the test fiber;
xi represents the elasto-optical coefficient of the test fiber;
Δt represents the amount of temperature change.
The difference in reflected center wavelengths of the test fiber and the reference fiber is represented by equation 3:
bringing equations 1 and 2 into equation 3, and the reflection center wavelengths of the reference optical fiber and the test optical fiber are approximately equal, that is, the wavelength drift amounts of the reference optical fiber and the test optical fiber generated along with the temperature change are consistent, so that equation 4 can be obtained:
namely, the difference value of the reflection center wavelength of the test optical fiber and the reference optical fiber is only related to the change of the hydrogen concentration, the fluctuation of the ambient temperature is eliminated, and the probe test signal packaged based on the method is not influenced by the temperature fluctuation.
The foregoing examples merely represent specific embodiments of the present application, which are described in more detail and are not to be construed as limiting the scope of the present application. It should be noted that, for those skilled in the art, several variations and modifications can be made without departing from the technical solution of the present application, which fall within the protection scope of the present application.
This background section is provided to generally present the context of the present invention and the work of the presently named inventors, to the extent it is described in this background section, as well as the description of the present section as not otherwise qualify as prior art at the time of filing, are neither expressly nor impliedly admitted as prior art against the present invention.

Claims (10)

1. A hydrogen sensor probe utilizing a reference fiber bragg grating, comprising:
the optical fiber testing device comprises a testing optical fiber and a reference optical fiber, wherein a Bragg grating area is arranged in each of the testing optical fiber and the reference optical fiber, and a cladding of the Bragg grating area is thinned after corrosion; uniformly coating the periphery of a Bragg grating area in the test optical fiber;
the test optical fiber and the reference optical fiber are sealed into a whole, and are coupled and connected together through an optical fiber coupling branching device;
and the fiber bragg grating demodulator demodulates and analyzes the spectrum signals after being coupled by the fiber bragg grating coupling branching device.
2. A hydrogen sensor probe using a reference fiber grating according to claim 1, wherein the cladding of the bragg grating region of the test and reference fibers is thinned by hydrofluoric acid etching to increase the sensitivity of the fiber to strain.
3. A hydrogen sensor probe using a reference fiber bragg grating according to claim 1, wherein the test fiber and the reference fiber each employ a single mode fiber bragg grating;
the cladding outside diameter of the non-corroded area of the test optical fiber and the reference optical fiber is 125 mu m, the diameter of the fiber core of the optical fiber is 8-10 mu m, the length of the Bragg grating area is 10mm, the reflection center wavelength of the optical fiber grating is 1510-1590 nm, the reflectivity is more than 90%, the 3dB bandwidth is 0.22nm, and the side mode suppression ratio is 18-22dB.
4. A hydrogen sensor probe using a reference fiber bragg grating according to claim 2, wherein the cladding of the bragg grating region of the test fiber and the reference fiber has an outer diameter of 20-50 μm after being etched by hydrofluoric acid.
5. The hydrogen sensor probe using a reference fiber bragg grating according to claim 1, wherein a Ti film, a PdAg alloy film and a Pd film are sequentially coated around the bragg grating region in the test fiber.
6. A hydrogen sensor probe using a reference fiber bragg grating according to claim 5, wherein said Ti film has a thickness of 5-10nm;
the thickness of the PdAG alloy film is 50-500nm;
the thickness of the Pd film is 5-20nm.
7. The hydrogen sensor probe using a reference fiber bragg grating according to claim 1, wherein the test fiber and the reference fiber are encapsulated in a stainless steel sleeve, and the tail is sealed with epoxy glue.
8. The preparation method of the hydrogen sensor probe by using the reference fiber bragg grating is characterized by comprising the following steps:
step S1: preprocessing two single-mode fiber gratings;
step S2: taking the pretreated single-mode fiber gratings as a substrate, and uniformly coating the periphery of a Bragg grating area of one single-mode fiber grating;
step S3: taking a coated single-mode fiber grating as a test fiber, taking an uncoated single-mode fiber grating as a reference fiber, sealing the test fiber and the reference fiber into a whole, and coupling and connecting the test fiber and the reference fiber together through a fiber coupling branching device;
step S4: and demodulating and analyzing the spectrum signals after being coupled by the fiber coupling branching device through the fiber grating demodulator.
9. The method for preparing a hydrogen sensor probe using a reference fiber bragg grating according to claim 8, wherein a bragg grating region is provided inside the single-mode fiber bragg grating;
the preprocessing in step S1 includes:
corroding and thinning the cladding of the Bragg grating area by adopting hydrofluoric acid;
the plating film in the step S2 includes:
uniformly plating Ti films, pdAG alloy films and Pd films on the periphery of the Bragg grating area in sequence by adopting a magnetron sputtering mode;
the step S3 includes:
packaging the test optical fiber and the reference optical fiber into a stainless steel sleeve, and sealing the tail part by adopting epoxy resin glue;
the test optical fiber and the reference optical fiber are connected to the optical fiber coupling branching device, and the optical fiber coupled by the optical fiber coupling branching device is connected to the optical fiber grating demodulator.
10. The method for preparing a hydrogen sensor probe using a reference fiber bragg grating according to claim 9, wherein the cladding of the fiber bragg grating has an outer diameter of 125 μm, the fiber core has a diameter of 8-10 μm, the bragg grating region has a length of 10mm, the fiber bragg grating has a reflection center wavelength of 1510-1590 nm, a reflectivity of >90%, a 3dB bandwidth of 0.22nm, and a side mode suppression ratio of 18-22dB;
the outer diameter of the cladding of the Bragg grating area is 20-50 mu m after being corroded by hydrofluoric acid;
the thickness of the Ti film is 5-10nm, the thickness of the PdAG alloy film is 50-500nm, and the thickness of the Pd film is 5-20nm.
CN202310358379.2A 2023-04-06 2023-04-06 Hydrogen sensor probe utilizing reference fiber bragg grating and preparation method thereof Pending CN116448681A (en)

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