CN103048270B - Method for preparing high-sensitivity probe of fiber Bragg grating hydrogen sensor - Google Patents
Method for preparing high-sensitivity probe of fiber Bragg grating hydrogen sensor Download PDFInfo
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- CN103048270B CN103048270B CN201210555986.XA CN201210555986A CN103048270B CN 103048270 B CN103048270 B CN 103048270B CN 201210555986 A CN201210555986 A CN 201210555986A CN 103048270 B CN103048270 B CN 103048270B
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- fiber grating
- hydrogen gas
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Abstract
The invention relates to a method for preparing a high-sensitivity probe of a fiber Bragg grating (FBG) hydrogen sensor. The method comprises the following steps: bonding an FBG with a glass substrate, wherein a Ti (Titanium) film is deposited on the FBG, a groove is etched in the glass substrate, and a grating region of the FBG is located in the center of the groove; uniformly mixing a modified WO3-Pt composite hydrogen-sensitive material with de-ionized water, coating the mixture in the groove, and uniformly covering the grating region of the FBG; and drying the WO3-Pt composite hydrogen-sensitive material, and encapsulating the glass substrate and the FBG, on which the deposited Ti film is deposited, in a porous Ti pipe so as to obtain the high-sensitivity probe of the FBG hydrogen sensor. According to the method for preparing the high-sensitivity probe of the FBG hydrogen sensor, contents of a WO3 phase and a catalyst Pt in the hydrogen-sensitive material are controlled through thermal treatment; the temperature sensitivity enhancement is performed on the Ti film of a protective layer plated on the FBG, thereby improving the sensitivity and stability of the sensor; and the method is significant to the practicality of the FBG hydrogen sensor.
Description
Technical field
The present invention relates to Optical Fider Hybrogen Sensor preparation technology, be specifically related to preparation technology and the encapsulation technology of fiber grating hydrogen gas sensor probe.
Background technology
Owing to having, volume is little, the advantage such as essential safety and electromagnetism interference and become study hotspot for Optical Fider Hybrogen Sensor in recent years.Current Optical Fider Hybrogen Sensor is mainly divided into disappearance field pattern, microlens type, F-P interfere type, surface ion resonance type and grating type optical fiber.Relative to the Optical Fider Hybrogen Sensor of other types, fiber-optic grating sensor has Large Copacity monitoring capability owing to adopting wavelength as restituted signal, and fiber grating hydrogen gas sensor can adopt the method with reference to grating to carry out temperature compensation, thus can improve degree of accuracy and the stability of sensor measurement.
WO
3be a kind of excellent gas sensitive, can react with multiple reducibility gas under the effect of catalyzer.By control WO
3phase structure and the type of catalyzer, WO hydrogen to good selectivity and sensitivity can be prepared
3-Pt composite hydrogen gas sensitive material.By WO
3-Pt composite hydrogen gas sensitive material combines with the fiber grating of enhanced sensitivity, utilizes WO
3-Pt composite hydrogen gas sensitive material and hydrogen reaction liberated heat, changed the centre wavelength of fiber grating, obtained the concentration of hydrogen by the change of detection fiber raster center wavelength.WO
3-the impact of micromechanism on hydrogen performance of Pt composite hydrogen gas sensitive material has vital role: on the one hand can by optimizing WO
3-phase structure and the lowest detection limit becoming to assign to improve hydrogen sensitivity and reduction density of hydrogen of Pt composite hydrogen gas sensitive material; The sensitivity that temperature sensitizing improves sensor further can be carried out on the other hand to fiber grating.Utilize the WO of modification
3-Pt composite hydrogen gas sensitive material prepares sensing probe with combining of enhanced sensitivity fiber grating, and carries out practical significant to this fiber grating hydrogen gas sensor of protectiveness encapsulation.
Summary of the invention
The object of the invention is to provide the preparation method of a kind of high-sensitivity optical fiber grating hydrogen gas sensor probe.
The present invention seeks to be realized by following technical proposals:
A kind of
the preparation method of high-sensitivity optical fiber grating hydrogen gas sensor probe, its
step is:to deposit the fiber grating of Ti film together with etching reeded substrate of glass and boning, and the grid region of fiber grating is positioned at the central authorities of groove; By modification WO
3-Pt composite hydrogen gas sensitive material mixes with deionized water in rear coating groove, and covers the grid region part of fiber grating equably; Dry WO
3after-Pt composite hydrogen gas sensitive material, by described substrate of glass together with depositing the optical fiber Bragg grating encapsulation of Ti film in porous Ti pipe, namely obtain
high-sensitivity optical fiber grating hydrogen gas sensor is popped one's head in.
One of the present invention
the preparation method of high-sensitivity optical fiber grating hydrogen gas sensor probe, comprise the steps:
1), WO
3prepared by-Pt composite hydrogen gas sensitive material: utilize ion exchange process to prepare wolframic acid colloidal sol, by wolframic acid colloidal sol through centrifugal, mix with chloroplatinic acid after washed with de-ionized water, after drying, put into high temperature furnace at 250 DEG C-360 DEG C thermal treatment 1h-8h, general heat treatment temperature is 315 DEG C, and heat treatment time is 1h, obtains WO
3-Pt composite hydrogen gas sensitive material, wherein W:Pt mol ratio is between 1:1 ~ 8.9:1;
2) 2), by fiber grating ultrasonic cleaning 30 minutes in absolute ethyl alcohol, then ultrasonic cleaning 20 minutes in deionized water, after dry with uviol lamp baking, puts into coating machine cavity sputtered with Ti film, Ti film thickness 10nm-200 μm;
3), by the fiber grating after plated film be fixed in the groove etching reeded substrate of glass, make grid region part be positioned at the central authorities of groove, have encapsulation groove respectively at groove two ends, the optical fiber at fiber grating two ends is arranged in encapsulation groove; To the two ends optical fiber Shi Hanzhang in fiber grating grid region, be coated in encapsulation groove with resistant to elevated temperatures glue, after glue solidifies completely, coated optical fibre grating just secures;
4), by step 1) WO
3the responsive powder of-Pt composite hydrogen gas mixes in the groove of rear coated glass substrate with deionized water, and covers the grid region part of fiber grating equably, and dry, wherein W:Pt mol ratio is between 1:1 ~ 8.9:1;
5), by substrate of glass together with being coated with WO
3the plating Ti film fiber grating part of-Pt composite hydrogen gas sensitive material, put into porous Ti pipe (long for 6cm, inside diameter be 3.4mm, outer dia is the porous Ti pipe of 4mm), optical fiber stretches out from the two ends of Ti pipe, with high temperature resistant glue, the optical fiber at substrate of glass two ends and porous Ti pipe are fixed together, namely obtain
high-sensitivity optical fiber grating hydrogen gas sensor is popped one's head in.
Of the present invention
in technical scheme, the fiber grating of described fiber grating or removal unit subcontract layer, its diameter is between 16 μm-125 μm.
Of the present invention
in technical scheme, the equivalent material of described Ti is Cr, Ni, W, Al, Cu, Pt or Au; When using Cr, Ni, W, Al, Cu material, at the glass capillary that coated optical fibre grating grid region cover 2cm is long, be then together fixed in substrate of glass groove, then apply WO
3-Pt composite sensitive material.
Of the present invention
in technical scheme, porous Ti manages or substitutes with porous ptfe tube, fritted glass steel pipe, porous ceramic pipe or porous stainless steel.
6, of the present invention
in technical scheme, substrate of glass can with the Ti metallic substrates of same size, silicate ceramics substrate, teflon or pure SiO
2substrate substitutes.
Of the present invention
in technical scheme, substrate of glass size is length 1-8mm, wide 1-5mm, thick 0.5-3mm; The size of the groove of substrate of glass sets according to the size of substrate, between length 1-3mm, wide 0.4-4mm, dark 0.1-2mm;
Of the present invention
in technical scheme, described high temperature resistant glue is EPOXY-353ND-A and B (Chinese name heat-curable epoxy resin A and B), is be coated on encapsulation groove and grating two ends fiber section after 10:1 stirs according to mass ratio A:B.
The present invention will optimize the WO of composition and phase structure
3-Pt composite hydrogen gas sensitive material combines with the fiber grating through temperature sensitizing and prepares the high-sensitivity optical fiber grating hydrogen gas sensor that can detect low-concentration hydrogen and pop one's head in; Pass through WO
3the optimization of-Pt composite hydrogen gas sensitive material phase structure and composition, it is made to have obvious thermal effect at 100ppm hydrogen, thus change the temperature of environment, under certain density of hydrogen, temperature reaches balance, utilizes the temperature sensitivity of fiber grating the concentration of hydrogen indirectly can be detected.
High-sensitivity optical fiber grating hydrogen gas sensor probe of the present invention, principle of work is: in fiber Bragg grating (FBG) demodulator, light source sends stable broadband light, is arrived be coated with WO by coupling mechanism
3the fiber grating of-Pt composite hydrogen gas sensitive material, the light of certain wavelength is reflexed to fiber Bragg grating (FBG) demodulator by this fiber grating.When sensing probe is placed on the atmosphere of hydrogen of variable concentrations, WO
3-Pt composite hydrogen gas sensitive material and hydrogen reaction, release heat and reach balance, change the temperature around enhanced sensitivity fiber grating, the centre wavelength of enhanced sensitivity fiber grating is changed, and the high sensitivity being realized density of hydrogen by the change of the centre wavelength detecting enhanced sensitivity fiber grating reflected light is accurately measured.
Sensor fibre in the present invention adopts single-mode fiber, use phase mask plate method, the ultraviolet light of generation is sent by excimer laser, when through mask plate diffraction, zero order diffracted light is attenuated to lower than transmission power 3%, and first-order diffraction is added or subtracts each other and be maximized, account for about 35% of whole transmission power respectively.First-order diffraction striped interferes, and interference fringe is radiated on fiber core, makes illuminated portion fiber core refractive index that permanent change occur, and forms grid region at the exposed portion of 8mm.Making a collection of centre wavelength by identical technique is fiber grating near 1300nm or 1550nm.Have reliability by the fiber grating standby by phase mask plate legal system high, reflectivity, more than 90%, can improve the enhancing greatly of detection signal.
In order to improve WO
3the hydrogen of-Pt composite hydrogen gas sensitive material is active, WO
3at 315 DEG C, heat-treat 1h, containing noncrystalline structure as much as possible in making its thing mutually, increase WO simultaneously
3in-Pt composite hydrogen gas sensitive material, the content of catalyst Pt is to improve hydrogen activity further; In order to overcome WO
3-Pt composite hydrogen gas sensitive material is directly combined with fiber grating and holds caducous shortcoming, fiber grating is fixed in the reeded substrate of glass of etching, groove has more coarse surface, by between composite hydrogen gas sensitive material coating groove and fiber grating, and can by WO
3-Pt composite hydrogen gas sensitive material is well fixed on around fiber grating; Depositing Ti film on fiber grating, can improve the temperature control of fiber grating on the one hand, to improve the sensitivity of sensor further, can play the effect of diaphragm on the other hand, and protection fiber grating is to improve the permanance of sensor; The substrate of glass and fiber grating that are coated with composite hydrogen gas sensitive material are together encapsulated in porous Ti pipe to play a protective role to sensor sensing part.
Accompanying drawing explanation
Fig. 1, be hydrogen gas sensor of the present invention probe in hydrogen sensitive material, fiber grating and substrate of glass assemble schematic diagram
Fig. 2, be hydrogen gas sensor of the present invention probe in substrate of glass and optical fiber Bragg grating encapsulation schematic diagram
Fig. 3, be hydrogen gas sensor of the present invention probe in porous Ti tubular construction schematic diagram
Fig. 4, be deposited the grid region structure enlarged diagram of the fiber grating of Ti film in hydrogen gas sensor of the present invention probe
Wherein: 1-porous Ti manages, 2-substrate of glass, 3-optical fiber, 4-is high temperature resistant glue, 5-hydrogen sensitive material, 6-deposited the fiber grating of Ti film, and 7-encapsulates groove, 8-groove, the grid region of 9-fiber grating, the covering of 10-optical fiber, the fibre core of 11-optical fiber, 12-Ti film.
Embodiment
Below in conjunction with accompanying drawing, the preparation method to the high-sensitivity optical fiber grating hydrogen gas sensor probe of invention is described in further detail.
High-sensitivity optical fiber grating hydrogen gas sensor sonde configuration of the present invention as Figure 1-4.It is produced as follows:
1), utilize ion exchange process to prepare wolframic acid colloidal sol, by wolframic acid colloidal sol through centrifugal, mix with chloroplatinic acid after washed with de-ionized water, after drying, put into high temperature furnace thermal treatment 1h at 315 DEG C of temperature, obtain WO
3-Pt composite hydrogen gas sensitive material, wherein W:Pt mol ratio is between 1:1 to 8.9:1, and the higher catalytic effect of Pt content is better; In order to WO
3containing amorphous phase WO as much as possible in-Pt composite hydrogen gas sensitive material
3, in heat treatment process, temperature is low as far as possible, remains between 250 DEG C to 360 DEG C, and the heat treatment temperature of concrete setting is determined according to the moisture of drying in rear material, and generally setting process temperature is 315 DEG C, and heat treatment time is 1h;
2), by fiber grating ultrasonic cleaning 30 minutes in absolute ethyl alcohol, then ultrasonic cleaning 20 minutes in deionized water, after dry with uviol lamp baking, puts into coating machine cavity sputtered with Ti film 12, Ti film as diaphragm, can play and strengthen responsive to temperature effect on the one hand on the other hand; Erode away the groove 8 of long 2cm, wide 2mm and dark 0.5mm long for 5cm, wide substrate of glass 2 centre the hydrofluorite for 3mm, thick 1mm, groove 8 can as hydrogen sensitive material 5 and the container of fiber grating 6 that deposited (plating) Ti film; Corrode the encapsulation groove 7 of long 1.5cm, wide 0.6mm, dark 0.5mm respectively at the two ends of groove 8, the effect of encapsulation groove 7 can be fixed in groove 8 by optical fiber horizontal; The fiber grating 6 having plated Ti film is put into groove 8, makes grid region part be positioned at the central authorities of groove 8, make the optical fiber at two ends be arranged in encapsulation groove 7; To two ends optical fiber 3 Shi Hanzhang in the grid region of fiber grating, by heat-curable epoxy resin A and B(EPOXY-353ND-A mixed up and B) stir according to the A:B ratio that is 1:10 after be coated in encapsulation groove 7, after glue solidifies completely, just complete the fixing of fiber grating;
3), a certain amount of WO is got
3-Pt composite hydrogen gas sensitive material, after mixing, is coated in the grid region part of the fiber grating of groove 8 in centrifuge tube with deionized water, then with heat gun by WO
3moisture in-Pt composite hydrogen gas sensitive material is dried, and this completes the fixing of hydrogen sensitive material 5;
4), substrate of glass 2 is put into together with plating Ti film fiber grating 6 part of coating hydrogen sensitive material 5 the porous Ti pipe 1 that length is 6cm, inside diameter is 3.4mm, outer dia is 4mm; optical fiber stretches out from the two ends of porous Ti pipe 1; the two ends of the POROUS TITANIUM pipe that high temperature resistant glue is coated in; after glue solidifies completely; the optical fiber 3 at substrate of glass two ends is fixed together with POROUS TITANIUM pipe 1; porous Ti pipe plays a protective role to sensor probe part, this completes the preparation of high-sensitivity optical fiber grating hydrogen gas sensor probe.
Claims (7)
1. a preparation method for high-sensitivity optical fiber grating hydrogen gas sensor probe, is characterized in that method step is: will deposit the fiber grating of Ti film together with etching reeded substrate of glass and boning, and the grid region of fiber grating is positioned at the central authorities of groove; By modification WO
3-Pt composite hydrogen gas sensitive material mixes with deionized water in rear coating groove, and covers the grid region part of fiber grating equably; Dry WO
3after-Pt composite hydrogen gas sensitive material, by described substrate of glass together with depositing the optical fiber Bragg grating encapsulation of Ti film in porous Ti pipe, namely obtaining high-sensitivity optical fiber grating hydrogen gas sensor probe, specifically comprising the steps:
1), WO
3prepared by-Pt composite hydrogen gas sensitive material: utilize ion exchange process to prepare wolframic acid colloidal sol, by wolframic acid colloidal sol through centrifugal, mix after washed with de-ionized water with chloroplatinic acid, after drying, puts into high temperature furnace at 250 DEG C-360 DEG C thermal treatment 1h-8h, obtains WO
3-Pt composite hydrogen gas sensitive material, wherein W:Pt mol ratio is between 1:1 ~ 8.9:1;
2), by fiber grating ultrasonic cleaning 30 minutes in absolute ethyl alcohol, then ultrasonic cleaning 20 minutes in deionized water, after dry with uviol lamp baking, puts into coating machine cavity sputtered with Ti film, Ti film thickness 10nm-200 μm;
3), by the fiber grating after plated film be fixed in the groove etching reeded substrate of glass, make grid region part be positioned at the central authorities of groove, have encapsulation groove respectively at groove two ends, the optical fiber at fiber grating two ends is arranged in encapsulation groove; To the two ends optical fiber Shi Hanzhang in fiber grating grid region, be coated in encapsulation groove with high temperature resistant glue, after glue solidifies completely, coated optical fibre grating just secures;
4), by step 1) WO
3be coated in the groove of substrate of glass after-Pt composite hydrogen gas sensitive material mixes with deionized water, and cover the grid region part of fiber grating equably, dry, wherein W:Pt mol ratio is between 1:1 ~ 8.9:1;
5), by substrate of glass together with being coated with WO
3the plating Ti film fiber grating part of-Pt composite hydrogen gas sensitive material, put into porous Ti pipe, optical fiber stretches out from the two ends of Ti pipe, with high temperature resistant glue, the optical fiber at substrate of glass two ends and porous Ti pipe is fixed together, i.e. obtained high-sensitivity optical fiber grating hydrogen gas sensor probe.
2. the preparation method of a kind of high-sensitivity optical fiber grating hydrogen gas sensor probe according to claim 1, it is characterized in that: the fiber grating of described fiber grating or removal unit subcontract layer, its diameter is between 16 μm-125 μm.
3. the preparation method of a kind of high-sensitivity optical fiber grating hydrogen gas sensor probe according to claim 1, is characterized in that: the equivalent material of described Ti is Cr, Ni, W, Al, Cu, Pt or Au; When using Cr, Ni, W, Al, Cu material, at the glass capillary that coated optical fibre grating grid region cover 2cm is long, be then together fixed in substrate of glass groove, then apply WO
3-Pt composite sensitive material.
4. the preparation method of a kind of high-sensitivity optical fiber grating hydrogen gas sensor probe according to claim 1, is characterized in that: porous Ti manages or substitutes with porous ptfe tube, fritted glass steel pipe, porous ceramic pipe or porous stainless steel.
5. the preparation method of a kind of high-sensitivity optical fiber grating hydrogen gas sensor probe according to claim 1, is characterized in that: substrate of glass can with the Ti metallic substrates of same size, silicate ceramics substrate, teflon or pure SiO
2substrate substitutes.
6. the preparation method of a kind of high-sensitivity optical fiber grating hydrogen gas sensor probe according to claim 1, is characterized in that: substrate of glass size is length 1-8mm, wide 1-5mm, thick 0.5-3mm; The size of the groove of substrate of glass sets according to the size of substrate, between length 1-3mm, wide 0.4-4mm, dark 0.1-2mm.
7. the preparation method of a kind of high-sensitivity optical fiber grating hydrogen gas sensor probe according to claim 1, it is characterized in that: the heat treatment temperature described in step 1) is 315 DEG C, heat treatment time is 1h.
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CA2768261A1 (en) * | 2009-07-16 | 2011-01-20 | Hamidreza Alemohammad | Optical fibre sensor and methods of manufacture |
CN101871885A (en) * | 2010-06-08 | 2010-10-27 | 中国计量学院 | Manufacture method of tilted fiber grating hydrogen sensor based on optical catalytic oxidation |
CN102175619B (en) * | 2011-02-16 | 2013-02-06 | 武汉理工大学 | Multi-layer composite sensitive film optical fiber hydrogen sensing probe and manufacturing method thereof |
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