CN111947697A - Novel fiber Bragg grating hydrogen sensor and manufacturing method - Google Patents
Novel fiber Bragg grating hydrogen sensor and manufacturing method Download PDFInfo
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- CN111947697A CN111947697A CN202010854469.7A CN202010854469A CN111947697A CN 111947697 A CN111947697 A CN 111947697A CN 202010854469 A CN202010854469 A CN 202010854469A CN 111947697 A CN111947697 A CN 111947697A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 120
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- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 28
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- FYFFGSSZFBZTAH-UHFFFAOYSA-N methylaminomethanetriol Chemical compound CNC(O)(O)O FYFFGSSZFBZTAH-UHFFFAOYSA-N 0.000 claims description 3
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- 230000004044 response Effects 0.000 description 11
- 239000013307 optical fiber Substances 0.000 description 8
- 230000035945 sensitivity Effects 0.000 description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
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- 229910052731 fluorine Inorganic materials 0.000 description 2
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D5/00—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable
- G01D5/26—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light
- G01D5/32—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light with attenuation or whole or partial obturation of beams of light
- G01D5/34—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light with attenuation or whole or partial obturation of beams of light the beams of light being detected by photocells
- G01D5/353—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light with attenuation or whole or partial obturation of beams of light the beams of light being detected by photocells influencing the transmission properties of an optical fibre
- G01D5/35306—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light with attenuation or whole or partial obturation of beams of light the beams of light being detected by photocells influencing the transmission properties of an optical fibre using an interferometer arrangement
- G01D5/35309—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light with attenuation or whole or partial obturation of beams of light the beams of light being detected by photocells influencing the transmission properties of an optical fibre using an interferometer arrangement using multiple waves interferometer
- G01D5/35316—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light with attenuation or whole or partial obturation of beams of light the beams of light being detected by photocells influencing the transmission properties of an optical fibre using an interferometer arrangement using multiple waves interferometer using a Bragg gratings
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a new fiber Bragg grating hydrogen sensor and a manufacturing method thereof, and the new fiber Bragg grating hydrogen sensor manufacturing method is characterized in that: the method comprises the following steps: step A, pretreatment of fiber bragg gratings; step B, assembly of a polydopamine layer: assembling the fiber Bragg grating surface after acid corrosion to obtain a polydopamine coating, wherein the polydopamine coating corresponds to a fiber Bragg grating region; step C, assembling a metal palladium membrane; d, assembling the super-hydrophobic breathable film: coating a layer of super-hydrophobic breathable film on the surface of the fiber Bragg grating hydrogen sensor loaded with polydopamine and metal palladium film; vacuum drying to obtain the fiber Bragg grating hydrogen sensor loaded with polydopamine, a metal palladium membrane and a super-hydrophobic breathable film; the invention can be widely applied to the fields of energy, chemical engineering, biochemical detection and the like.
Description
Technical Field
The invention relates to a hydrogen sensor, in particular to a novel fiber Bragg grating hydrogen sensor and a manufacturing method thereof.
Background
Hydrogen energy is a renewable energy source with high combustion heat value, cleanness and no pollution, and is considered as an ideal energy source for replacing conventional fossil fuels. The government work report and the Chinese blue book for the development of infrastructure of hydrogen energy industry clearly put forward the facility construction of charging, hydrogenation and the like, and plan the development route of the hydrogen energy industry. The safety of hydrogen production, storage, transportation and other processes must be ensured while the popularization of hydrogen energy is realized. The hydrogen atoms are atoms with the smallest volume in all elements, so that the density and the quality of the hydrogen atoms are also the smallest at normal temperature and normal pressure, the hydrogen atoms are easy to leak in the production, storage and transportation processes, and when a certain concentration value is accumulated in a closed space or in a ventilation bad condition, the hydrogen atoms are extremely inflammable and explosive, cause accidents and threaten the safety of lives and properties of people. Therefore, the development of the real-time online detection technology of the hydrogen concentration in the environment eliminates the explosion hidden danger caused by hydrogen leakage in the production, storage and transportation processes, and is the key for realizing the safe, reliable and universal application of hydrogen energy.
The sensors currently used for detecting the concentration of hydrogen mainly include electrochemical sensors, semiconductor sensors, catalytic combustion sensors and optical fiber sensors. Among these, electrochemical and semiconductor sensors use electrical signals for detection, presenting a potential discharge hazard. The catalytic combustion type sensor utilizes noble metals such as platinum and the like to catalyze the combustion reaction of hydrogen and oxygen, realizes the detection of the hydrogen concentration by detecting a temperature signal, and belongs to the field of blind fire work. When the two types of sensors are used for detecting the concentration of hydrogen, the risk of ignition and explosion exists. The optical fiber sensor uses optical signals for detection, has no discharge phenomenon and hidden fire generation, has intrinsic safety, and has the remarkable advantages of small geometric size, higher sensitivity, high response speed, distributed measurement and the like, thereby becoming the most promising sensor in the hydrogen concentration real-time online detection technology.
The existing optical fiber hydrogen sensor mainly comprises an optical fiber grating type hydrogen sensor, an interference type hydrogen sensor, a micro-lens type hydrogen sensor and an evanescent field type hydrogen sensor. The hydrogen sensor based on the fiber Bragg grating has the advantages of high response sensitivity, fast response time, strong anti-interference capability and quasi-distributed detection. Therefore, the fiber grating type hydrogen sensor becomes a research hotspot of a hydrogen leakage safety detection technology. Although the fiber grating type sensor has the advantages, the existing fiber grating type sensor still has the problem that the surface hydrogen-sensitive palladium film is easy to crack and fall off after hydrogen absorption and release circulation for many times. Particularly in a high-humidity environment, bubbling, cracking, and peeling of the palladium film are further accelerated. This is mainly because when the palladium membrane absorbs hydrogen, an alpha phase and a beta phase are generated, and the alpha phase and the beta phase have larger difference of lattice expansion coefficients, so that the palladium membrane is often peeled and cracked after undergoing hydrogen absorption-desorption hydrogen cycles, and the service life of the sensor is influenced. Particularly, after water molecules are attached to the surface of the palladium film, the local diffusion speed of hydrogen atoms is limited and hydrogen competitive adsorption is generated, so that the local stress between the palladium film and the optical fiber is increased, and further the structural damage of the FBG hydrogen sensor is caused. Therefore, it is very important to research a preparation method of the hydrogen sensitive film which can overcome cracking and shedding and enhance the bonding force between the hydrogen sensitive film and the substrate and prepare the hydrogen sensor which stably operates in a high-humidity environment.
Disclosure of Invention
The invention aims to provide a novel fiber Bragg grating hydrogen sensor and a manufacturing method thereof.
The technical scheme of the invention is as follows: a new method for manufacturing a fiber Bragg grating hydrogen sensor is characterized by comprising the following steps: the method comprises the following steps:
step A, fiber grating pretreatment: in order to improve the response sensitivity of the FBG sensor to hydrogen, firstly, the fluorine resin coating layer on the surface of the fiber Bragg grating is removed, then the fiber Bragg grating is cleaned, and finally the fiber Bragg grating is corroded for later use by acid liquid with certain concentration.
Step B, assembly of a polydopamine layer: in order to efficiently adsorb palladium ions in a palladium chloride solution to form a palladium core and enhance the adhesion strength of the palladium core on the surface of an optical fiber, assembling the surface of the optical fiber Bragg grating subjected to acid corrosion by utilizing a dopamine rapid deposition polymerization method to obtain a polydopamine coating; the coating position of the polydopamine coating corresponds to the grating region of the fiber Bragg grating.
The steps of assembling to obtain the polydopamine coating are as follows:
and step B1, weighing a certain amount of tris, dissolving in deionized water to prepare the obtained tris solution, and then adjusting the pH of the tris solution to be alkaline.
And step B2, weighing a certain amount of dopamine hydrochloride, dissolving the dopamine hydrochloride into the trihydroxymethylaminomethane buffer solution obtained in the step B1, mixing and uniformly stirring to obtain a dopamine hydrochloride solution.
And step B3, adding a certain amount of copper sulfate pentahydrate and hydrogen peroxide into the dopamine hydrochloride solution prepared in the step B2 in sequence, and mixing and uniformly stirring to obtain the rapid dopamine deposition solution.
And step B4, soaking the fiber Bragg grating processed in the step A into the dopamine rapid deposition solution obtained in the step B3, and depositing for a certain time, so that the poly-dopamine coating is assembled on the surface of the fiber Bragg grating.
And step B5, drying the assembled fiber Bragg grating loaded with the polydopamine coating in a vacuum drying oven.
Step C, assembling the metal palladium membrane: in order to assemble the surface of the fiber Bragg grating loaded with the polydopamine coating to obtain a compact and uniform metal palladium membrane, the metal palladium membrane is assembled by the following steps:
step C1, preparing a palladium chloride hydrochloric acid solution: weighing a certain amount of palladium chloride, dissolving the palladium chloride in HCl solution, mixing and stirring uniformly, and preparing to obtain palladium chloride hydrochloric acid solution.
Step C2, preparing a sodium borohydride solution: weighing a certain amount of NaBH4Dissolving in deionized water, mixing and stirring uniformly, and preparing to obtain a sodium borohydride solution.
Step C3, soaking the fiber Bragg grating loaded with the polydopamine coating prepared in the step B5 into the palladium chloride hydrochloric acid solution prepared in the step C1, and heating in a water bath for a certain time; and then immersing the immersed fiber Bragg grating into a sodium borohydride solution, and alternately immersing for a plurality of times to obtain the fiber Bragg grating loaded with the polydopamine coating and the palladium nanoparticle film.
Step C4, preparing chemical plating solution:
step C42, measuring ammonia water, dissolving the ammonia water in deionized water, stirring, weighing disodium ethylene diamine tetraacetate, dissolving the disodium ethylene diamine tetraacetate in the ammonia water solution, and magnetically stirring to obtain a mixed solution of the disodium ethylene diamine tetraacetate and the ammonia water;
c43, dropwise adding the palladium chloride hydrochloric acid solution into the mixed solution of the disodium ethylene diamine tetraacetate and the ammonia water, magnetically stirring, and stably complexing for a certain time; obtaining a plating solution;
step C44, preparing hydrazine hydrate reduction solution;
step C45, dropwise adding the hydrazine hydrate reducing solution into the plating solution prepared in the step C43, and magnetically stirring to obtain chemical plating solution;
step C5, chemically plating a metal palladium film: heating chemical plating solution in a water bath, immersing the fiber Bragg grating loaded with the polydopamine and palladium nanoparticle film in the chemical plating solution, performing chemical deposition for a certain time, finally immersing in deionized water to remove residual chemical plating solution, and performing vacuum drying to obtain the fiber Bragg grating hydrogen sensor loaded with the polydopamine and metal palladium film; the palladium metal membrane is located on the outer surface of the polydopamine coating.
D, assembling the super-hydrophobic breathable film: the stability and the accuracy of the operation of the fiber Bragg grating hydrogen sensor in a high-humidity environment are enhanced; coating a layer of super-hydrophobic breathable film on the surface of the fiber Bragg grating hydrogen sensor loaded with polydopamine and metal palladium film; and (3) drying in vacuum to obtain the fiber Bragg grating hydrogen sensor loaded with polydopamine, the metal palladium membrane and the super-hydrophobic breathable membrane, wherein the super-hydrophobic breathable membrane is positioned on the outer surface of the metal palladium membrane.
According to the preferable scheme of the novel method for manufacturing the fiber Bragg grating hydrogen sensor, the mass percentages of the palladium chloride, the hydrochloric acid, the ethylene diamine tetraacetic acid, the ammonia water and the hydrazine hydrate reducing solution are as follows: 0.16 to 0.2 weight percent of palladium chloride, 0.5 to 0.6 weight percent of hydrochloric acid, 4 to 5 weight percent of disodium ethylene diamine tetraacetate, 20 to 22 weight percent of ammonia water and 0.3 to 0.4 weight percent of hydrazine hydrate.
According to the preferable scheme of the novel method for manufacturing the fiber bragg grating hydrogen sensor, the dopamine hydrochloride and tris buffer solution in the step B2 are as follows by mass percent: 0.19 to 0.21 weight percent of dopamine hydrochloride and 0.55 to 0.65 weight percent of tris (hydroxymethyl) aminomethane.
A new fiber Bragg grating hydrogen sensor comprises a fiber Bragg grating with a surface fluororesin coating removed, and is characterized in that: the surface of the fiber Bragg grating is loaded with a polydopamine coating, and the coating position of the polydopamine coating corresponds to the grating region of the fiber Bragg grating; the surface of the polydopamine coating is loaded with a metal palladium membrane, and the surface of the metal palladium membrane is coated with a super-hydrophobic breathable film.
The novel fiber Bragg grating hydrogen sensor and the manufacturing method have the advantages that the fiber Bragg grating hydrogen sensor prepared by the method can realize quick and accurate detection of hydrogen leakage in the environment and enhance the stability and accuracy of the detection of the hydrogen sensor in a high-humidity environment; the method is simple and can be widely applied to the fields of energy, chemical engineering, biochemical detection and the like.
Drawings
Fig. 1 is a schematic structural diagram of a new fiber bragg grating hydrogen sensor according to the present invention.
FIG. 2a is a graph showing the response of the hydrogen sensor of the present invention to 1-3-5% hydrogen concentration.
FIG. 2b is the sensitivity of the hydrogen sensor of the present invention to detect hydrogen at concentrations of 0-5%.
FIG. 3 is a graph of the response of the hydrogen sensor of the present invention to 5% hydrogen in a humidity environment of 20-80% RH.
Detailed Description
Referring to fig. 1, a new method for manufacturing a fiber bragg grating hydrogen sensor is characterized in that: the method comprises the following steps:
step A, fiber grating pretreatment: in order to improve the response sensitivity of the FBG sensor to hydrogen, firstly, the fluorine resin coating layer on the surface of the fiber Bragg grating is removed by about 18mm, then the grating area part is sequentially immersed in absolute ethyl alcohol and deionized water for ultrasonic oscillation cleaning for 10min, and finally the fiber Bragg grating is corroded to 5-65 μm by hydrofluoric acid with a certain concentration for later use.
Step B, assembly of a polydopamine layer: in order to efficiently adsorb palladium ions in a palladium chloride solution to form a palladium core and enhance the adhesion strength of the palladium core on the surface of an optical fiber, assembling the surface of the fiber Bragg grating corroded by hydrofluoric acid by utilizing a dopamine rapid deposition polymerization method to obtain a polydopamine coating; the coating position of the polydopamine coating corresponds to the grating region of the fiber Bragg grating.
The steps of assembling to obtain the polydopamine coating are as follows:
step B1, weighing a certain amount of 0.1817g of tris, dissolving in 30mL of deionized water to prepare a 50mmol/L tris solution, and then adjusting the pH of the tris solution to 8.5.
And step B2, weighing a certain amount of 60mg dopamine hydrochloride, dissolving the dopamine hydrochloride into the trihydroxymethylaminomethane buffer solution obtained in the step B1, mixing and uniformly stirring to obtain a 2mg/mL dopamine hydrochloride solution.
And step B3, weighing a certain amount of 23.9415mg of blue vitriol and 30% of hydrogen peroxide 59uL in sequence, adding into the dopamine hydrochloride solution prepared in the step B2, mixing and stirring uniformly to obtain the rapid dopamine deposition solution.
And step B4, soaking the fiber Bragg grating processed in the step A into the dopamine rapid deposition solution obtained in the step B3, and depositing for a certain time of 10-40 mm, so that a polydopamine coating with the thickness of about 9-36nm can be assembled on the surface of the fiber Bragg grating region.
And step B5, placing the assembled fiber Bragg grating loaded with the polydopamine coating in a vacuum drying oven, and drying for 30min at 60 ℃.
Step C, assembling the metal palladium membrane: in order to assemble the surface of the fiber Bragg grating loaded with the polydopamine coating to obtain a compact and uniform metal palladium membrane, the metal palladium membrane is assembled by the following steps:
step C1, preparing a palladium chloride hydrochloric acid solution: a certain amount of 0.1329g of palladium chloride is weighed and dissolved in 25mL of 0.2mol/L HCl solution, and the solution is mixed and stirred uniformly to obtain 10mmol/L of palladium chloride hydrochloric acid solution.
Step C2 preparing sodium borohydride solution: a certain amount of 0.0076g of NaBH is weighed4Dissolving in 20mL deionized water, mixing and stirring uniformly, and preparing to obtain 10mmol/L sodium borohydride solution which is used as the preparation.
And step C3, soaking the fiber Bragg grating loaded with the polydopamine coating prepared in the step B5 into the palladium chloride hydrochloric acid solution prepared in the step C1, and heating in a water bath at 45 ℃ for 3 min. And then immersing the immersed fiber bragg grating into a sodium borohydride solution for 1min, and repeating the immersion for a plurality of times, for example, 3-5 times, so as to prepare the fiber bragg grating loaded with the polydopamine coating and the palladium nanoparticle film.
Step C4, preparing chemical plating solution:
c41, preparing 5mL of 0.24mol/L diluted hydrochloric acid, weighing a certain amount of 40mg of palladium chloride, dissolving in the diluted hydrochloric acid, and ultrasonically oscillating for 10min to obtain the palladium chloride hydrochloric acid solution.
Step C42, measuring 3mL of ammonia water, dissolving the ammonia water in 5mL of deionized water, stirring for 10min, and weighing disodium ethylene diamine tetraacetate Na2Dissolving EDTA1g in ammonia water solution, and magnetically stirring for 10min to obtain mixed solution of disodium ethylenediamine tetraacetic acid and ammonia water.
C43, dropwise adding the palladium chloride hydrochloric acid solution prepared in the step C41 into a mixed solution of disodium ethylenediamine tetraacetic acid and ammonia water, magnetically stirring for 10min, and stably complexing for a certain time of 2 h; and obtaining the plating solution.
And step C44, sucking 80uL of 80% hydrazine hydrate and dissolving in 4.92mL of ultrapure water to prepare 5mL of hydrazine hydrate reduction solution with the concentration of 0.08mol/5 mL.
And C45, dropwise adding the hydrazine hydrate reducing solution into the plating solution prepared in the step C43, magnetically stirring for 50min, and fixing the volume to 20mL, namely preparing the chemical plating solution.
Step C5, chemically plating a metal palladium film: heating chemical plating solution from normal temperature water bath to 45 ℃, then immersing the fiber Bragg grating loaded with the polydopamine/palladium nanoparticle film into the chemical plating solution, after chemical deposition for 1-3min, finally immersing into deionized water to remove residual chemical plating solution, and then performing vacuum drying at 60 ℃ for 30min to obtain the fiber Bragg grating hydrogen sensor loaded with the polydopamine coating and the metal palladium film; the palladium metal membrane is located on the outer surface of the polydopamine coating.
D, assembling the super-hydrophobic breathable film: the stability and the accuracy of the operation of the fiber Bragg grating hydrogen sensor in a high-humidity environment are enhanced; coating a layer of silicon oxide super-hydrophobic film on the surface of a fiber Bragg grating hydrogen sensor loaded with a polydopamine/palladium film; vacuum drying at 60-80 deg.C for 20min to obtain the fiber Bragg grating hydrogen sensor loaded with polydopamine coating, metal palladium film and super-hydrophobic coating. The super-hydrophobic breathable film is positioned on the outer surface of the metal palladium film.
In the specific embodiment, in the steps C41 to C45 of preparing the electroless plating solution, the mass percentages of the palladium chloride, the hydrochloric acid, the disodium edetate, the ammonia water and the hydrazine hydrate reducing solution are as follows: 0.16 to 0.2 weight percent of palladium chloride, 0.5 to 0.6 weight percent of hydrochloric acid, 4 to 5 weight percent of disodium ethylene diamine tetraacetate, 20 to 22 weight percent of ammonia water and 0.3 to 0.4 weight percent of hydrazine hydrate; preferably 0.187 wt% palladium chloride, 0.552 wt% hydrochloric acid, 4.683 wt% disodium ethylenediamine tetraacetic acid, 21.352 wt% ammonia water and 0.386 wt% hydrazine hydrate.
The mass percentage of the dopamine hydrochloride and the tris buffer solution in the step B2 is as follows: 0.19 to 0.21 weight percent of dopamine hydrochloride and 0.55 to 0.65 weight percent of tris (hydroxymethyl) aminomethane. Preferably 0.198% wt of dopamine hydrochloride and 0.601% wt of tris (hydroxymethyl) aminomethane.
In order to detect the hydrogen-sensitive response performance of the fiber bragg grating hydrogen sensor based on the polydopamine/palladium membrane, the real-time cyclic response condition of the FBG hydrogen sensor to 1-3-5% concentration hydrogen and the detection sensitivity to 0-5% concentration hydrogen are tested experimentally, and the experimental results are shown in fig. 2(a) and fig. 2 (b). As can be seen from FIG. 2(a), when hydrogen gas with a concentration of 1-3-5% is sequentially introduced into the gas chamber at a flow rate of 1000sccm, the center wavelength of the FBG rapidly increases and drifts, and the drift amplitude of the center wavelength increases with the increase of the hydrogen gas concentration. This is because the metal palladium film can adsorb hydrogen to expand, which causes the FBG gate region to be strained and the gate pitch to change, and further causes the FBG center wavelength to shift. Over timeAnd increasing, wherein the central wavelength of the FBG is gradually stabilized and does not continue to increase in the detection process of the hydrogen with the same concentration. This is because the palladium membrane becomes increasingly saturated with hydrogen and no longer causes FBG deformation and central wavelength drift. The FBG center wavelength can again be returned to the origin when the hydrogen is removed. And the amount of center wavelength drift increases as the concentration of detected hydrogen increases. Fig. 2(b) shows the central wavelength shift of FBG hydrogen sensors loaded with poly-dopamine/palladium membrane superhydrophobic coatings at different hydrogen concentrations of 0-5%. The FBG hydrogen sensor is at 1-5% H2The response is approximately linear in the concentration range, and the response sensitivity can reach 10.7 pm/% H. Research results show that the fiber Bragg grating based on the polydopamine/palladium film can accurately, continuously and repeatedly monitor hydrogen concentration change information.
In order to test the operation condition of the FBG hydrogen sensor based on the polydopamine/palladium membrane/super-hydrophobic coating in a high-humidity environment, the test condition of the FBG hydrogen sensor on 5% concentration hydrogen at relative humidity of 20-80% RH is experimentally tested, and the experimental result is shown in fig. 3. As can be seen from fig. 3, the FBG hydrogen sensor can respond to 5% concentration hydrogen gas consistently at different relative humidities, and has no sensor desensitization. Research results show that the fiber Bragg grating hydrogen sensor based on the polydopamine/palladium membrane/super-hydrophobic coating can accurately and stably monitor hydrogen concentration change information in a high-humidity environment.
A new hydrogen sensor of fiber Bragg grating comprises the fiber Bragg grating without surface fluororesin coating, wherein the fiber Bragg grating comprises a fiber cladding 1, a fiber core 2 and a fiber Bragg grating area 3; the surface of the fiber Bragg grating is rapidly deposited with a polydopamine coating 4 with strong adhesiveness and reducibility, and the polydopamine coating corresponds to the fiber Bragg grating region 3; and a hydrogen-sensitive metal palladium membrane 5 is chemically plated and deposited on the surface of the polydopamine coating 4, and a super-hydrophobic breathable film 6 is coated on the surface of the metal palladium membrane 5. The polydopamine coating has the function of adsorbing palladium ions and primarily reducing the palladium ions into palladium simple substances. The metal palladium film is used as a hydrogen sensitive material, generates volume expansion after absorbing hydrogen and is used for hydrogen sensitive detection of the fiber Bragg grating hydrogen sensor. The super-hydrophobic breathable film has the function of isolating a high-humidity environment and preventing water molecules from interfering the palladium film to adsorb hydrogen.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (4)
1. A new method for manufacturing a fiber Bragg grating hydrogen sensor is characterized by comprising the following steps: the method comprises the following steps:
step A, fiber grating pretreatment: firstly, removing a fluororesin coating layer on the surface of the fiber Bragg grating, then cleaning the fiber Bragg grating, and finally corroding the fiber Bragg grating for later use by utilizing acid liquid with certain concentration;
step B, assembly of a polydopamine layer: assembling the surface of the fiber Bragg grating subjected to acid corrosion by utilizing a dopamine rapid deposition polymerization method to obtain a polydopamine coating; the polydopamine coating corresponds to a fiber Bragg grating region;
the steps of assembling to obtain the polydopamine coating are as follows:
step B1, weighing a certain amount of tris, dissolving in deionized water to prepare an obtained tris solution, and then adjusting the pH of the tris solution to be alkaline;
b2, weighing a certain amount of dopamine hydrochloride, dissolving the dopamine hydrochloride in the trihydroxymethylaminomethane buffer solution obtained in the step B1, mixing and uniformly stirring to obtain a dopamine hydrochloride solution;
step B3, adding a certain amount of copper sulfate pentahydrate and hydrogen peroxide into the dopamine hydrochloride solution prepared in the step B2 in sequence, mixing and uniformly stirring to obtain a rapid dopamine deposition solution;
step B4, immersing the fiber Bragg grating processed in the step A into the dopamine rapid deposition solution obtained in the step B3, and depositing for a certain time, so that a poly-dopamine coating is assembled on the surface of the fiber Bragg grating;
step B5, placing the assembled fiber Bragg grating loaded with the polydopamine coating in a vacuum drying oven for drying;
step C, assembling the metal palladium membrane:
step C1, preparing a palladium chloride hydrochloric acid solution: weighing a certain amount of palladium chloride, dissolving the palladium chloride in HCl solution, mixing and stirring uniformly, and preparing to obtain palladium chloride hydrochloric acid solution;
step C2 preparing sodium borohydride solution: weighing a certain amount of NaBH4Dissolving in deionized water, mixing and stirring uniformly, and preparing to obtain a sodium borohydride solution;
step C3, soaking the fiber Bragg grating loaded with the polydopamine coating prepared in the step B5 into the palladium chloride hydrochloric acid solution prepared in the step C1, and heating in a water bath for a certain time; then immersing the immersed fiber Bragg grating into a sodium borohydride solution, and alternately immersing for a plurality of times to obtain the fiber Bragg grating loaded with the polydopamine coating and the palladium nanoparticle film;
step C4, preparing chemical plating solution:
step C42, measuring ammonia water, dissolving the ammonia water in deionized water, stirring, weighing disodium ethylene diamine tetraacetate, dissolving the disodium ethylene diamine tetraacetate in the ammonia water solution, and magnetically stirring to obtain a mixed solution of the disodium ethylene diamine tetraacetate and the ammonia water;
c43, dropwise adding the palladium chloride hydrochloric acid solution into the mixed solution of the disodium ethylene diamine tetraacetate and the ammonia water, magnetically stirring, and stably complexing for a certain time; obtaining a plating solution;
step C44, preparing hydrazine hydrate reduction solution;
step C45, dropwise adding the hydrazine hydrate reducing solution into the plating solution prepared in the step C43, and magnetically stirring to obtain chemical plating solution;
step C5, chemically plating a metal palladium film: heating chemical plating solution in a water bath, immersing the fiber Bragg grating loaded with the polydopamine and palladium nanoparticle film in the chemical plating solution, performing chemical deposition for a certain time, finally immersing in deionized water to remove residual chemical plating solution, and performing vacuum drying to obtain the fiber Bragg grating hydrogen-sensitive sensor loaded with the polydopamine and metal palladium film; the metal palladium membrane is positioned on the outer surface of the polydopamine coating;
d, assembling the super-hydrophobic breathable film: coating a layer of super-hydrophobic breathable film on the surface of the fiber Bragg grating hydrogen sensor loaded with polydopamine and metal palladium film; and (3) vacuum drying to obtain the fiber Bragg grating hydrogen sensor loaded with the polydopamine coating, the metal palladium membrane and the super-hydrophobic breathable membrane, wherein the super-hydrophobic breathable membrane is positioned on the outer surface of the metal palladium membrane.
2. The method for manufacturing a new fiber bragg grating hydrogen sensor according to claim 1, wherein: the mass percentages of the palladium chloride, the hydrochloric acid, the ethylene diamine tetraacetic acid, the ammonia water and the hydrazine hydrate reducing solution are as follows: 0.16 to 0.2 weight percent of palladium chloride, 0.5 to 0.6 weight percent of hydrochloric acid, 4 to 5 weight percent of disodium ethylene diamine tetraacetate, 20 to 22 weight percent of ammonia water and 0.3 to 0.4 weight percent of hydrazine hydrate.
3. The method for manufacturing a new fiber bragg grating hydrogen sensor according to claim 1, wherein: the mass percentage of the dopamine hydrochloride and the tris buffer solution in the step B2 is as follows: 0.19 to 0.21 weight percent of dopamine hydrochloride and 0.55 to 0.65 weight percent of tris (hydroxymethyl) aminomethane.
4. A new fiber Bragg grating hydrogen sensor comprises a fiber Bragg grating with a surface fluororesin coating removed, and is characterized in that: the surface of the fiber Bragg grating is loaded with a polydopamine coating, and the polydopamine coating corresponds to a grating region of the fiber Bragg grating; and a metal palladium membrane is loaded on the surface of the polydopamine coating, and a super-hydrophobic breathable film is coated on the surface of the metal palladium membrane.
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