CN103048270A - 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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- CN103048270A CN103048270A CN201210555986XA CN201210555986A CN103048270A CN 103048270 A CN103048270 A CN 103048270A CN 201210555986X A CN201210555986X A CN 201210555986XA CN 201210555986 A CN201210555986 A CN 201210555986A CN 103048270 A CN103048270 A CN 103048270A
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- fiber grating
- optical fiber
- groove
- substrate
- glass
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- 239000000835 fiber Substances 0.000 title claims abstract description 68
- 239000001257 hydrogen Substances 0.000 title claims abstract description 60
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 60
- 239000000523 sample Substances 0.000 title claims abstract description 32
- 125000004435 hydrogen atoms Chemical class data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [H]* 0.000 title abstract 8
- 239000000463 material Substances 0.000 claims abstract description 44
- 239000000758 substrate Substances 0.000 claims abstract description 39
- 239000011521 glass Substances 0.000 claims abstract description 34
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 4
- 238000007669 thermal treatment Methods 0.000 claims abstract description 4
- 239000003365 glass fiber Substances 0.000 claims description 46
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 42
- -1 compound hydrogen Chemical class 0.000 claims description 31
- 238000002360 preparation method Methods 0.000 claims description 19
- 238000005538 encapsulation Methods 0.000 claims description 16
- 239000003292 glue Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- CMPGARWFYBADJI-UHFFFAOYSA-L Tungstic acid Chemical compound 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- 239000011540 sensing material Substances 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N silicate Chemical compound 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[O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials 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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
Advantage such as Optical Fider Hybrogen Sensor volume is little owing to having, essential safety and anti-electromagnetic interference (EMI) etc. becomes study hotspot in recent years.Optical Fider Hybrogen Sensor mainly is divided into disappearance field pattern, microlens type, F-P interfere type, surface ion resonance type and grating type optical fiber at present.Optical Fider Hybrogen Sensor with respect to other types, fiber-optic grating sensor is owing to adopting wavelength to have large capacity monitoring ability as restituted signal, and the fiber grating hydrogen gas sensor can adopt with reference to the method for grating and carry out temperature compensation, thereby can improve degree of accuracy and the stability of sensor measurement.
WO
3Be a kind of good gas sensitive, under the effect of catalyzer, can react with multiple reducibility gas.By control WO
3Phase structure and the type of catalyzer, can prepare the WO that hydrogen is had good selectivity and sensitivity
3The compound hydrogen sensitive material of-Pt.With WO
3The compound hydrogen sensitive material of-Pt combines with the fiber grating of enhanced sensitivity, utilizes WO
3The compound hydrogen sensitive material of-Pt and hydrogen reaction liberated heat change the centre wavelength of fiber grating, obtain the concentration of hydrogen by the variation of detection fiber raster center wavelength.WO
3-The micromechanism of the compound hydrogen sensitive material of Pt has vital role to the impact of hydrogen performance: on the one hand can be by optimizing WO
3-The phase structure of the compound hydrogen sensitive material of Pt and the lowest detection limit that becomes to assign to improve to hydrogen sensitivity and reduction density of hydrogen; Can carry out the sensitivity that temperature sensitizing further improves sensor to fiber grating on the other hand.Utilize the WO of modification
3The preparation sensing probe that combines of the compound hydrogen sensitive material of-Pt and enhanced sensitivity fiber grating, and carry out practical significant to this fiber grating hydrogen gas sensor of protectiveness encapsulation.
Summary of the invention
The object of the invention provides a kind of preparation method of high-sensitivity optical fiber grating hydrogen gas sensor probe.
The present invention seeks to realize by following technical proposals:
A kind of
The preparation method of high-sensitivity optical fiber grating hydrogen gas sensor probe, its
Step is:The fiber grating that deposits the Ti film is bondd with the reeded substrate of glass of etching, and the grid region of fiber grating is positioned at the central authorities of groove; With modification WO
3The compound hydrogen sensitive material of-Pt and deionized water mix in the rear coating groove, and cover equably the grid region part of fiber grating; Oven dry WO
3Behind the compound hydrogen sensitive material of-Pt, with described substrate of glass together with the optical fiber Bragg grating encapsulation that deposits the Ti film in porous Ti pipe, namely obtain
High-sensitivity optical fiber grating hydrogen gas sensor probe
Of the present invention a kind of
The preparation method of high-sensitivity optical fiber grating hydrogen gas sensor probe, comprise the steps:
1), WO
3The compound hydrogen sensitive material preparation of-Pt: utilize ion exchange process to prepare wolframic acid colloidal sol, wolframic acid colloidal sol process is centrifugal, mix with chloroplatinic acid after the washed with de-ionized water, after through oven dry, put into high temperature furnace at 250 ℃ of-360 ℃ of thermal treatment 1h-8h, general heat treatment temperature is 315 ℃, and heat treatment time is 1h, obtains WO
3The compound hydrogen sensitive material of-Pt, wherein the W:Pt mol ratio is between 1:1 ~ 8.9:1;
2) 2), with fiber grating ultrasonic cleaning 30 minutes in absolute ethyl alcohol, then cleaned 20 minutes in deionized water for ultrasonic, after doing with the uviol lamp baking, put into coating machine cavity sputtered with Ti film, Ti film thickness 10nm-200 μ m;
3), the fiber grating behind the plated film is fixed in the groove of the reeded substrate of glass of etching, make the grid region part be positioned at the central authorities of groove, at the groove two ends encapsulation groove is arranged respectively, the optical fiber at fiber grating two ends is arranged in the encapsulation groove; Two ends optical fiber to the fiber grating grid region applies prestress, is coated in the encapsulation groove with resistant to elevated temperatures glue, and after glue solidified fully, the coated optical fibre grating was just fixing;
4), with step 1) WO
3The responsive powder of the compound hydrogen of-Pt and deionized water mix in the groove of rear coated glass substrate, and cover equably the grid region part of fiber grating, oven dry, and wherein the W:Pt mol ratio is between 1:1 ~ 8.9:1;
5), with substrate of glass together with being coated with WO
3The plating Ti film fiber grating part of the compound hydrogen sensitive material of-Pt, put into porous Ti pipe (the long 6cm of being, inside diameter are that 3.4mm, outer dia are 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 make
High-sensitivity optical fiber grating hydrogen gas sensor probe
Of the present invention
In the technical scheme, the fiber grating of described fiber grating or removal part covering, its diameter is between 16 μ m-125 μ m.
Of the present invention
In the 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 long glass capillary of coated optical fibre grating grid region cover 2cm, then together be fixed in the substrate of glass groove, apply again WO
3-Pt composite sensing material.
Of the present invention
In the technical scheme, porous Ti pipe or alternative with porous ptfe tube, fritted glass steel pipe, porous ceramic pipe or porous stainless steel.
6, of the present invention
In the technical scheme, substrate of glass can be used Ti metallic substrates, silicate ceramics substrate, teflon or the pure SiO of same size
2Substrate substitutes.
Of the present invention
In the technical scheme, the substrate of glass size is length 1-8mm, wide 1-5mm, thick 0.5-3mm; The size of the groove of substrate of glass is set according to the size of substrate, between length 1-3mm, wide 0.4-4mm, the dark 0.1-2mm;
Of the present invention
In the technical scheme, described high temperature resistant glue is EPOXY-353ND-A and B (Chinese name heat-curable epoxy resin A and B), is to 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
3The compound hydrogen sensitive material of-Pt combines with the fiber grating of process temperature sensitizing and prepares the high-sensitivity optical fiber grating hydrogen gas sensor probe that can detect low-concentration hydrogen; Pass through WO
3The optimization of-Pt compound hydrogen sensitive material phase structure and composition, make it at 100ppm hydrogen obvious thermal effect be arranged, thereby change the temperature of environment, temperature reaches balance under certain density of hydrogen, 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: light source sends stable broadband light in the fiber Bragg grating (FBG) demodulator, arrives by coupling mechanism and has applied WO
3The fiber grating of the compound hydrogen sensitive material of-Pt, 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
3The compound hydrogen sensitive material of-Pt and hydrogen reaction, emit heat and reach balance, change enhanced sensitivity fiber grating temperature on every side, the centre wavelength of enhanced sensitivity fiber grating is changed, realize that by the variation that detects the catoptrical centre wavelength of enhanced sensitivity fiber grating the high sensitivity of density of hydrogen accurately measures.
Sensor fibre among the present invention adopts single-mode fiber, use the phase mask plate method, send the ultraviolet light of generation by excimer laser, when seeing through the mask plate diffraction, zero order diffracted light is attenuated to and is lower than 3% of transmission power, and first-order diffraction addition or subtract each other is maximized, and accounts for respectively about 35% of whole transmission power.The first-order diffraction striped interferes, and interference fringe is radiated on the fiber core, makes the illuminated portion fiber core refractive index that permanent change occur, in the exposed portion formation grid region of 8mm.Making a collection of centre wavelength by identical technique is near 1300nm or the 1550nm fiber grating.By having the reliability height with the standby fiber grating of phase mask plate legal system, reflectivity can improve the greatly enhancing of detection signal more than 90%.
In order to improve WO
3The hydrogen of the compound hydrogen sensitive material of-Pt is active, WO
3Under 315 ℃, heat-treat 1h, make and contain noncrystalline structure as much as possible in its phase, increase simultaneously WO
3The content of catalyst Pt is active with further raising hydrogen in the compound hydrogen sensitive material of-Pt; In order to overcome WO
3The compound hydrogen sensitive material of-Pt and fiber grating are directly in conjunction with holding caducous shortcoming, fiber grating is fixed on the reeded substrate of glass of etching, groove has more coarse surface, and compound hydrogen sensitive material is applied between groove and the fiber grating, can be with WO
3The compound hydrogen sensitive material of-Pt well be fixed on fiber grating around; Depositing Ti film on fiber grating, one side can improve the temperature control of fiber grating, with the sensitivity of further raising sensor, can play on the other hand the effect of diaphragm, and the protection fiber grating is to improve the permanance of sensor; Together be encapsulated in porous Ti pipe and can partly play a protective role to sensor sensing having applied the substrate of glass of compound hydrogen sensitive material and fiber grating.
Description of drawings
Fig. 1, be that hydrogen sensitive material in the hydrogen gas sensor of the present invention probe, fiber grating assemble synoptic diagram with substrate of glass
Fig. 2, be substrate of glass and optical fiber Bragg grating encapsulation synoptic diagram in the hydrogen gas sensor of the present invention probe
Fig. 3, be porous Ti tubular construction synoptic diagram in the hydrogen gas sensor of the present invention probe
Fig. 4, be the grid region structure enlarged diagram that has deposited the fiber grating of Ti film in the hydrogen gas sensor of the present invention probe
Wherein: 1-porous Ti pipe, the 2-substrate of glass, 3-optical fiber, the high temperature resistant glue of 4-, 5-hydrogen sensitive material, 6-have 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
Preparation method to the high-sensitivity optical fiber grating hydrogen gas sensor probe of invention is described in further detail below in conjunction with accompanying drawing.
High-sensitivity optical fiber grating hydrogen gas sensor sonde configuration of the present invention is shown in Fig. 1-4.It is produced as follows:
1), utilize ion exchange process to prepare wolframic acid colloidal sol, wolframic acid colloidal sol through centrifugal, is mixed with chloroplatinic acid after the washed with de-ionized water, after through oven dry, put into high temperature furnace thermal treatment 1h under 315 ℃ of temperature, obtain WO
3The compound hydrogen sensitive material of-Pt, wherein between the 8.9:1, the higher catalytic effect of Pt content is better at 1:1 for the W:Pt mol ratio; For WO
3Contain amorphous phase WO as much as possible in the compound hydrogen sensitive material of-Pt
3, temperature is low as far as possible in the heat treatment process, remains between 250 ℃ to 360 ℃, and the concrete heat treatment temperature of setting is decided according to the moisture in the rear material of oven dry, and setting generally speaking treatment temperature is 315 ℃, and heat treatment time is 1h;
2), with fiber grating ultrasonic cleaning 30 minutes in absolute ethyl alcohol, then cleaned 20 minutes in deionized water for ultrasonic, after doing with the uviol lamp baking, put into coating machine cavity sputtered with Ti film 12, the Ti film can as diaphragm, can play the effect of enhancing responsive to temperature on the one hand on the other hand; Long for 5cm, widely erode away the groove 8 of long 2cm, wide 2mm and dark 0.5mm with hydrofluorite in the middle of for the substrate of glass 2 of 3mm, thick 1mm, groove 8 can and deposit the container of the fiber grating 6 of (plating) Ti film as hydrogen sensitive material 5; Corrode respectively the encapsulation groove 7 of long 1.5cm, wide 0.6mm, dark 0.5mm at the two ends of groove 8, the effect of encapsulation groove 7 is can being fixed in the groove 8 optical fiber horizontal; The fiber grating 6 that has plated the Ti film is put into groove 8, make the 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; Two ends optical fiber 3 to the grid region of fiber grating applies prestress, with heat-curable epoxy resin A and B(EPOXY-353ND-A and the B that mixes up) be to be coated in after the ratio of 1:10 stirs in the encapsulation groove 7 according to A:B, after glue solidifies fully, just finished the fixing of fiber grating;
3), get a certain amount of WO
3The compound hydrogen sensitive material of-Pt after mixing with deionized water, is coated in the grid region part of the fiber grating of groove 8 in centrifuge tube, then with heat gun with WO
3The fixing of hydrogen sensitive material 5 so just finished in moisture oven dry in the compound hydrogen sensitive material of-Pt;
4), substrate of glass 2 being put into length together with plating Ti film fiber grating 6 parts that apply hydrogen sensitive material 5 is that 3.4mm, outer dia are the porous Ti pipe 1 of 4mm for 6cm, inside diameter; 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 fully; the optical fiber 3 at substrate of glass two ends is fixed together with POROUS TITANIUM pipe 1; porous Ti pipe partly plays a protective role to sensor probe, has so just finished the preparation of high-sensitivity optical fiber grating hydrogen gas sensor probe.
Claims (8)
1. the preparation method of a high-sensitivity optical fiber grating hydrogen gas sensor probe is characterized in that method step is: will deposit the fiber grating of Ti film with the reeded substrate of glass bonding of etching, and the grid region of fiber grating is positioned at the central authorities of groove; With modification WO
3The compound hydrogen sensitive material of-Pt and deionized water mix in the rear coating groove, and cover equably the grid region part of fiber grating; Oven dry WO
3Behind the compound hydrogen sensitive material of-Pt, with described substrate of glass together with the optical fiber Bragg grating encapsulation that deposits the Ti film in porous Ti pipe, namely obtain 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 is characterized in that, comprises the steps:
1), WO
3The compound hydrogen sensitive material preparation of-Pt: utilize ion exchange process to prepare wolframic acid colloidal sol, wolframic acid colloidal sol through centrifugal, is mixed with chloroplatinic acid after the washed with de-ionized water, after through oven dry, put into high temperature furnace at 250 ℃ of-360 ℃ of thermal treatment 1h-8h, obtain WO
3The compound hydrogen sensitive material of-Pt, wherein the W:Pt mol ratio is between 1:1 ~ 8.9:1;
2), with fiber grating ultrasonic cleaning 30 minutes in absolute ethyl alcohol, then cleaned 20 minutes in deionized water for ultrasonic, after doing with the uviol lamp baking, put into coating machine cavity sputtered with Ti film, Ti film thickness 10nm-200 μ m;
3), the fiber grating behind the plated film is fixed in the groove of the reeded substrate of glass of etching, make the grid region part be positioned at the central authorities of groove, at the groove two ends encapsulation groove is arranged respectively, the optical fiber at fiber grating two ends is arranged in the encapsulation groove; Two ends optical fiber to the fiber grating grid region applies prestress, is coated in the encapsulation groove with high temperature resistant glue, and after glue solidified fully, the coated optical fibre grating was just fixing;
4), with step 1) WO
3Be coated in the groove of substrate of glass after the compound hydrogen sensitive material of-Pt and deionized water mix, and cover equably the grid region part of fiber grating, oven dry, wherein the W:Pt mol ratio is between 1:1 ~ 8.9:1;
5), with substrate of glass together with being coated with WO
3The plating Ti film fiber grating part of the compound hydrogen sensitive material of-Pt, 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, and namely makes high-sensitivity optical fiber grating hydrogen gas sensor probe.
3. the preparation method of a kind of high-sensitivity optical fiber grating hydrogen gas sensor probe according to claim 1 and 2, it is characterized in that: the fiber grating of described fiber grating or removal part covering, its diameter is between 16 μ m-125 μ m.
4. the preparation method of a kind of high-sensitivity optical fiber grating hydrogen gas sensor probe according to claim 1 and 2, it 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 long glass capillary of coated optical fibre grating grid region cover 2cm, then together be fixed in the substrate of glass groove, apply again WO
3-Pt composite sensing material.
5. the preparation method of a kind of high-sensitivity optical fiber grating hydrogen gas sensor probe according to claim 1 and 2 is characterized in that: porous Ti pipe or alternative with porous ptfe tube, fritted glass steel pipe, porous ceramic pipe or porous stainless steel.
6. the preparation method of a kind of high-sensitivity optical fiber grating hydrogen gas sensor probe according to claim 1 and 2 is characterized in that: substrate of glass can be with Ti metallic substrates, silicate ceramics substrate, teflon or the pure SiO of same size
2Substrate substitutes.
7. the preparation method of a kind of high-sensitivity optical fiber grating hydrogen gas sensor probe according to claim 1 and 2, it is characterized in that: the substrate of glass size is length 1-8mm, wide 1-5mm, thick 0.5-3mm; The size of the groove of substrate of glass is set according to the size of substrate, between length 1-3mm, wide 0.4-4mm, the dark 0.1-2mm.
8. the preparation method of a kind of high-sensitivity optical fiber grating hydrogen gas sensor probe according to claim 2, it is characterized in that: the heat treatment temperature described in the step 1) is 315 ℃, heat treatment time is 1h.
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| CN104931458A (en) * | 2015-06-24 | 2015-09-23 | 中国计量学院 | MZI (Mach-Zehnder interferometer) hydrogen sensor based on fiber brag grating microcavity |
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| CN107037088A (en) * | 2016-02-03 | 2017-08-11 | 天津大学 | Carry platinum wolframic acid zinc nano material and its synthetic method |
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| CN108489901A (en) * | 2018-03-29 | 2018-09-04 | 武汉理工大学 | Optical fiber hydrogen detecting system based on New Hydrogen sensitive film |
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