CN104596939B - Twice silver plated fiber bragg grating gas sensor - Google Patents
Twice silver plated fiber bragg grating gas sensor Download PDFInfo
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- CN104596939B CN104596939B CN201510079405.3A CN201510079405A CN104596939B CN 104596939 B CN104596939 B CN 104596939B CN 201510079405 A CN201510079405 A CN 201510079405A CN 104596939 B CN104596939 B CN 104596939B
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Abstract
The invention discloses a twice silver plated fiber bragg grating gas sensor. A separation cavity is connected with a sensor fixing flange at the upper end through a flange fixing thread; a small hole is formed in the center of the sensor fixing flange; an optic fiber passes through the small hole; a silver plated FBG gas sensitive element is arranged at the lower end of the optic fiber; a streamline protective shell is arranged outside the silver plated FBG gas sensitive element; an equidistant spiral guide slot is engraved in the inner wall of the separation cavity; the bottom of the separation cavity is connected with a device with a spiral diversion hole through a fixed thread; the screw pitch of the device with the spiral diversion hole is same as that of the spiral guide slot in the separation cavity. In order to ensure the effective contact between the gas in well fluid and a gas sensitive film plating layer and correctly measure the concentration of the underground gas, oil-gas separation is carried out at first and then the gas content is detected through plating a sensitive material Ag film on a fiber bragg grating (FBG). By adopting a rotary separation principle and separating the gas and liquid phases by means of centrifugal force, the twice silver plated fiber bragg grating gas sensor has the advantages of being reasonable in design, simple in structure, convenient to operate, high in sensitivity and suitable for the real-time detection of low-concentration H2S gas and environment temperature in oil gas wells.
Description
Technical field
The invention belongs to technical field of optical fiber sensing is and in particular to be used for oil gas downhole detection low concentration hydrogen sulphide to a kind of
The secondary silver-plated fiber grating gas sensor of gas.
Background technology
With the development of petro chemical industry, inflammable, explosive, toxic gas species and coverage are obtained for increasing
Plus.These gases are producing, transport, use during once leak, it will cause be poisoned, fire or even explosion accident,
The safety of life and property of the serious harm people.Sour gas well gas blowout accident is along with hydrogen sulfide (h2The releasing of toxic gas such as s)
Put or burn, serious casualties, property loss can be caused and affect environment;The hydrogen sulfide gas detection of Oil/gas Well down-hole is oil
Gas field exploration, the difficulties of development field.Hydrogen sulfide gas sensing used in exploration of oil and gas field well logging at present, production logging
Device is mainly based on the traditional detection methods such as metal oxide, electrochemistry, catalytic combustion type, optical-mechanic one.Due to detection machine
Reason, sensor construction, performance and down-hole lay the impact of the factors such as difficulty, traditional h2S gas detection method is in well
Take test in laboratory after sampling or operation area environment and well head near zone are detected, the reality of down-hole difficult to realize
When detection.It is fast that fiber gas sensor has a response, high precision, and electromagnetism interference, corrosion-resistant, structure is simple, down-hole need not electricity
(light) source, selectivity is good, signal transmission attenuation is little, easy networking many advantages, is particularly suitable for being harmful in severe and hazardous environment
The detection of gas.
Content of the invention
In order to overcome existing traditional these hydrogen sulfide gas sensor to be unable to the defect of down-hole laying, the purpose of the present invention exists
In proposing a kind of secondary silver-plated fiber grating gas sensor: in order to allow gas in well liquid effectively to contact with air-sensitive film coating,
Accurately measure the concentration of mine gas, first have to carry out Oil-gas Separation, on this basis, by the upper plating of fiber grating (fbg)
Sensitive material ag film is detecting gas content.The present invention adopts rotating separation principle, and the effect relying on centrifugal force is carrying out gas-liquid
The separation of two-phase, has reasonable in design, structure and is simple and convenient to operate, sensitivity high it is adaptable under Oil/gas Well real-time detection low dense
The h of degree2S gas and environment temperature.
In order to achieve the above object, technical problem be the technical scheme is that
A kind of secondary silver-plated fiber grating gas sensor, includes disengagement chamber 5, disengagement chamber 5 pass through flange fixation screw thread 4 and
The sensor mounting flange 1 of upper end connects, and the center of sensor mounting flange 1 has aperture a, and optical fiber c passes through in aperture a,
The lower end of optical fiber c is silver-plated fbg gas sensor 2, and the outside of silver-plated fbg gas sensor 2 is streamlined protection shell 3, optical fiber c,
Silver-plated fbg gas sensor 2 and streamlined protection shell 3 constitute entirely streamlined sensing element b, and the inwall of disengagement chamber 5 is carved with
Away from spiral guide slot 6, the bottom of disengagement chamber 5 is passed through fixing screw thread 7 and is connected with the device d with spiral stream guidance hole 8, has spiral
The pitch of device d of pod apertures 8 is identical with disengagement chamber 5 inside spin gathering sill, 6 pitch, right on the excircle in spiral stream guidance hole 8
Claim to be dispersed with residual night tap 9.
The lower section at the cross framework center of described sensor mounting flange 1 is circular cone platform.
The length of described disengagement chamber 5 is 150-160mm, and external diameter is 130-140mm, wall thickness 10-15mm;Material is resistance to height
The corrosion resistant stainless steel of temperature.
Described silver-plated fbg gas sensor 2 length is 30-40mm, and coating film thickness is 12-15 μm.
Described streamlined protection shell 3 length is 50-60mm.
The pitch of described gathering sill 6 is 90-100mm.
Described silver-plated fbg gas sensor 2, its silver plating process is as follows:
(1) optical fiber fbg is immersed in the concentrated sulfuric acid, remove surface coating layer;After deionized water is rinsed then anhydrous with speckling with
The absorbent cotton of ethanol is cleaned repeatedly it is ensured that the coat of optical fiber surface is thoroughly got rid of;
(2) fbg removing overlay is put in glassware, add the agno3 solution of 0.1mol/l, addition guarantees
The fbg removing overlay is totally submerged, and instills 0.2mol/l naoh solution to tan precipitate, then is added dropwise over
0.2mol/l ammoniacal liquor, side edged rocks glassware, till the sediment until generating is completely dissolved just;
(3) instilling mass concentration in glassware is 10% glucose solution, adds the volume of glucose solution to account for always
The 3%-5% of liquor capacity, and container is placed in 50-60 DEG C of water-bath heating, now, silverskin on fbg plated surface, but thin
Film thickness is relatively thin, and uniformity is not good;
(4) in the agno of 0.1mol/l30.2mol/l naoh solution is added until tan precipitate occurs in solution, then
It is added dropwise over 0.2mol/l ammoniacal liquor, side edged rocks glassware, till the sediment until generating is completely dissolved just, by it
Ice bath cools down, then in temperature t=0 DEG C, adds the glucose solution accounting for cumulative volume 3%-8%, its mass concentration is
12%, the fbg of the surface of step (3) gained plated film is immersed, carries out second coating process, now can observe
To mixture color from faint yellow, be changed into red, then be changed into grey, the change of color represents and generates collargol and experience
Condensation process, completes silver plating process.
The feature of the present invention:
(1) due to h2S gas has hypertoxicity, therefore, realizes light concentration gas detection and warning seems very necessary.Light
Fine grating itself and h2S gas reaction is insensitive, thus the present invention be obtained using silver-plated film secondary on fiber grating highly sensitive
The h of degree2S gas sensor.
(2) present invention proposes one kind and detects h by plating sensitive material ag film secondary on fbg2The optical fiber gas of s gas
Dependent sensor structure, on the one hand to increase the uniformity of silverskin using secondary silver-plated preparation method, improves the spirit of gas sensor
Sensitivity;On the other hand h is ensured using special Oil-gas Separation, streamlined protection shelling machine2S gas is had with gas sensor
Effect contact, realizes the real-time detection of down-hole low concentration hydrogen sulphide gas.
Brief description
Fig. 1 is the structural representation of the present invention, and wherein Fig. 1-a is stereogram, and Fig. 1-b is sectional view.
Fig. 2 is the assembling schematic diagram of the present invention.
Fig. 3 is the structural representation of streamlined protection shell 3 in Fig. 1.
Fig. 4 is to fbg gas sensor 2 secondary film coating effect contrast figure, and wherein Fig. 4-a is design sketch silver-plated for the first time,
Fig. 4-b is second silver-plated design sketch.
Fbg peak power variation diagram before and after Fig. 5 adsorption of hydrogen sulfide.
Fig. 6 is the x-rd collection of illustrative plates after silver-plated gas sensor adsorption of hydrogen sulfide gas.
Specific embodiment
The present invention is described in more detail with each embodiment below in conjunction with the accompanying drawings, but the invention is not restricted to these enforcements
Example.
See figures.1.and.2, a kind of secondary silver-plated fiber grating gas sensor, including disengagement chamber 5, gas-liquid two-phase here
Carry out separating, disengagement chamber 5 is connected with sensor mounting flange 1 by the fixing screw thread 4 of flange, the center of sensor mounting flange 1
Have aperture a, optical fiber c passes through in aperture a, the lower end of optical fiber c is silver-plated fbg gas sensor 2, silver-plated fbg gas sensor 2
Outside is streamlined protection shell 3, the silver-plated fbg gas sensor 2 within protection, and can be to the gas after rotating separation
Liquid mixture carries out separating again so that separating gas to enter protection enclosure by air admission hole, effective with air-sensitive film coating
Contact;Optical fiber c, silver-plated fbg gas sensor 2 and streamlined protection shell 3 constitute entirely streamlined sensing element b, disengagement chamber 5
Inwall be carved with isometric helix gathering sill 6, the bottom of disengagement chamber 5 is passed through fixing screw thread 7 and is connected with the dress with spiral stream guidance hole 8
Put d, the well liquid that vertical ascent is ordered about in spiral stream guidance hole 8 produces rotary motion, have the pitch of device d in spiral stream guidance hole 8 with
Disengagement chamber 5 inside spin gathering sill, 6 pitch are identical, will effectively be converted into turning moment to the pressure separating cavity wall, guide fluid
Reaching at short notice needs rotary speed, and according to the difference of rate of flow of fluid under real well, pitch can do corresponding regulation,
Symmetrical residual night tap 9 on the excircle in spiral stream guidance hole 8.
The lower section at the cross framework center of described sensor mounting flange 1 is circular cone platform, plays guide functions, can allow stream
Discharge rapidly by the oil gas tap between cross framework for body.
The length of described disengagement chamber 5 is 150-160mm, and external diameter is 130-140mm, wall thickness 10-15mm;Material is resistance to height
The corrosion resistant stainless steel of temperature.
Described silver-plated fbg gas sensor 2 length is 30-40mm, and coating film thickness is 12-15 μm.
Described streamlined protection shell 3 length is 50-60mm.
The pitch of described gathering sill 6 is 90-100mm.
Described silver-plated fbg gas sensor 2, its silver plating process is as follows:
(1) optical fiber fbg is immersed in the concentrated sulfuric acid, remove surface coating layer;After deionized water is rinsed, then with speckling with no
The absorbent cotton of water-ethanol is cleaned repeatedly it is ensured that the coat of optical fiber surface is thoroughly got rid of;
(2) fbg removing overlay is put in glassware, add the agno3 solution of 0.1mol/l, addition guarantees
The fbg removing overlay is totally submerged, and instills 0.2mol/l naoh solution to tan precipitate, then is added dropwise over
0.2mol/l ammoniacal liquor, side edged rocks glassware, till the sediment until generating is completely dissolved just;
(3) instilling mass concentration in glassware is 10% glucose solution, adds the volume of glucose solution to account for always
The 3%-5% of liquor capacity, and container is placed in 50-60 DEG C of water-bath heating, now, silverskin on fbg plated surface, but thin
Film thickness is relatively thin, and uniformity is not good;
(4) in the agno of 0.1mol/l30.2mol/l naoh solution is added until tan precipitate occurs in solution, then
It is added dropwise over 0.2mol/l ammoniacal liquor, side edged rocks glassware, till the sediment until generating is completely dissolved just, by it
Ice bath cools down, then in temperature t=0 DEG C, adds the glucose solution accounting for cumulative volume 3%-8%, its mass concentration is
12%, the fbg of the surface of step (3) gained plated film is immersed, carries out second coating process, now can observe
To mixture color from faint yellow, be changed into red, then be changed into grey, the change of color represents and generates collargol and experience
Condensation process, completes silver plating process.Because condensation process silver-colored at low temperature is more slowly it is possible to preferably control silverskin
Thickness and the uniformity.
With reference to Fig. 3, there is air admission hole 3-1 at the middle part of streamlined protection shell 3, has raffinate tap 3-2 in its bottom;Rotation
Separate after gas-liquid mixture from below pass through streamlined protection shell 3, through flow dynamics analysis, most of gas can pass through into
Pore 3-1 enters enclosure, effectively contacts with air-sensitive film coating, realizes separating further of gas-liquid two-phase.Air admission hole is straight
Footpath is (3-5mm), and wall thickness is (1-2mm).Least a portion of liquid can enter inside containment vessel with gas, under pressure,
Flowed out by raffinate tap 3-2.Tap a diameter of (3-5mm), wall thickness is (1-2mm).
The course of work of the present invention is as follows:
Downhole fluid vertical ascent, enters spiral stream guidance hole 8, and the well liquid that it can order about vertical ascent produces rotary motion,
Rotation well liquid enters into disengagement chamber 5, the spiral guide slot 6 of disengagement chamber 5 inwall, the pitch phase in its pitch and spiral stream guidance hole 8
With it will effectively be converted into turning moment to the pressure separating cavity wall, and guiding fluid reaches needs rotation speed at short notice
Degree.For relative liquid, the less gas of density then concentrates near disengagement chamber 5 axis, wherein also mixes a small amount of liquid,
Now achieve the initial gross separation of gas-liquid two-phase.Remaining liquid oil gas tap between cross framework from flange 1 flows out and passes
Sensor.
Inside disengagement chamber 5, the gas mixing a small amount of liquid passes through streamlined protection shell 3, according to fluid mechanics principle,
Fluid is separated further, and a large amount of gases pass through air admission hole 3-1 and enter protection enclosure, by silver-plated fiber grating gas sensor
2 are detected, minimal amount of liquid also enters protection enclosure with gas, due to pressure effect, by raffinate tap
3-2 flows out.
According to different measuring demand, also silver-plated fiber grating down-hole gas sensor can be installed on two sleeve pipe linkings
Place, now the diameter of disengagement chamber 5 is suitable with casing diameter, sensor mounting flange 1, streamlined protection shell 3, spiral stream guidance hole
8 size needs to be designed according to specific casing diameter.
Under jsm 6309a type SEM, after Fig. 4 is fbg first time silver-plated film, amplify 900 times of picture;
After Fig. 5 is second silver-plated film of fbg, amplify 900 times of picture under jsm 6309a type SEM.
During the silver-plated film of fiber grating, remove the overlay at optical fiber fbg first with the concentrated sulfuric acid, single mode is mixed in germanium fbg employing
The product of the micro- Optical Sensing Limited in state Beijing, core diameter is 8.30 ± 0.05 μm, and cladding diameter is 125.0 ± 0.5 μm, applies
Coating type is acrylate, polyimide, and thickness is 245 ± 10 μm, and grating length is 10.0 ± 0.2mm, and reflectivity is
95%, wavelength is 1549.85nm, and 3db carries a width of 0.3nm.Optical fiber fbg central area 40mm is fixed on I shape optical fiber install
On support, support is immersed in the concentrated sulfuric acid, after static about 15min, remove surface coating layer;Deionized water rinses 5min, goes
Except fbg surface h+And so4 2-Ion;Repeatedly clean 2min with the absorbent cotton speckling with absolute ethyl alcohol it is ensured that the coat of optical fiber surface is thorough
Bottom is got rid of, and it is 30.0 ± 5.0mm that coat removes length.
The fbg removing overlay puts in the glassware of a diameter of 150mm, adds 2ml 0.1mo1/l agno3Molten
Liquid, adds 1-2 to drip the naoh solution of 0.2mol/l, now tan precipitate, then be added dropwise over 2mo1/l ammoniacal liquor, side edged
Weak vibrations glassware, till the sediment until generating is completely dissolved just.Finally, instill a little mass concentration 10%
Glucose solution, and container is placed on heating 15min in 50-60 DEG C of water-bath, now, fbg surface has plated silverskin, but silver-colored
Film relatively thin and uneven (as depicted in fig. 4-a).
In clean glassware, in the agno of 0.1mol/l30.2mol/l naoh solution is added until going out in solution
Existing tan precipitate, then it is added dropwise over 0.2mol/l ammoniacal liquor, side edged rocks glassware, and the sediment until generating is just complete
Till CL.It is cooled down in ice bath, in temperature t=0 DEG C, the glucose adding a little mass concentration to be 12% is molten
Liquid, silver-plated fbg is put in mixed solution, now it is observed that the color of mixture, from faint yellow, is changed into red,
Be changed into grey again, the change of color represent generate collargol and experience condensation process.Due to condensation silver-colored at low temperature
Journey is more slow it is possible to preferable control silver film thickness and the uniformity (as shown in Fig. 4-b), and thickness is 13.982um.
Silver-plated fbg gas sensor is placed in h2During s gaseous environment, it is deposited on ag atom and the h of cladding surface2S gas produces such as
Lower electrochemical reaction: 2ag+s--→ag2s+2e-
Silver-plated fbg gas sensor surface metal silver from a kind of bright typical metal surface, become turn to a kind of dark and not
Transparent material surface.The evanescent wave energy of incoming optical fiber reduces, the peak power also phase of silver-plated fbg gas sensor reflectance spectrum
Should reduce.Fig. 5 display absorption h2Fbg peak power change before and after s gas, curve a is higher for power before absorption, and curve b is to inhale
Attached power drop.
Fig. 6 is the x-rd collection of illustrative plates after silver-plated gas sensor adsorption of hydrogen sulfide gas, and 4 stronger peaks of in figure spread out for ags
Penetrate peak.To the from left to right the 2nd diffraction maximum analysis shows: curve a is the ags diffraction maximum collection of illustrative plates generating, curve b is standard diagram, two
It is preferable that person coincide.
Claims (7)
1. it is characterised in that including disengagement chamber (5), disengagement chamber (5) passes through method to a kind of secondary silver-plated fiber grating gas sensor
Blue fixing screw thread (4) is connected with the sensor mounting flange (1) of upper end, and the center of sensor mounting flange (1) has aperture
A (), optical fiber (c) passes through in aperture (a), and the lower end of optical fiber (c) is silver-plated fbg gas sensor (2), silver-plated fbg gas sensor
(2) outside is streamlined protection shell (3), optical fiber (c), silver-plated fbg gas sensor (2) and streamlined protection shell (3) structure
Become entirely streamlined sensing element (b), the inwall of disengagement chamber (5) is carved with isometric helix gathering sill (6), the bottom of disengagement chamber (5)
The device (d) with spiral stream guidance hole (8) is connected with by fixing screw thread (7), there is the device (d) in spiral stream guidance hole (8)
Pitch is identical with disengagement chamber (5) inside spin gathering sill (6) pitch, symmetrical residual on the excircle of spiral stream guidance hole (8)
Night tap (9);
There is air admission hole (3-1) at the middle part of streamlined protection shell (3).
2. a kind of secondary silver-plated fiber grating gas sensor according to claim 1 is it is characterised in that described sensing
The lower section at the cross framework center of device mounting flange (1) is circular cone platform.
3. a kind of secondary silver-plated fiber grating gas sensor according to claim 1 is it is characterised in that described separation
The length in chamber (5) is 150-160mm, and external diameter is 130-140mm, wall thickness 10-15mm;Material is the stainless of corrosion-and high-temp-resistant
Steel.
4. a kind of secondary silver-plated fiber grating gas sensor according to claim 1 is it is characterised in that described is silver-plated
Fbg gas sensor (2) length is 30-40mm, and coating film thickness is 12-15 μm.
5. a kind of secondary silver-plated fiber grating gas sensor according to claim 1 is it is characterised in that described streamline
Type protection shell (3) length is 50-60mm.
6. a kind of secondary silver-plated fiber grating gas sensor according to claim 1 is it is characterised in that described guiding
The pitch of groove (6) is 90-100mm.
7. a kind of secondary silver-plated fiber grating gas sensor according to claim 1 is it is characterised in that described is silver-plated
Fbg gas sensor (2), its silver plating process is as follows:
(1) optical fiber fbg is immersed in the concentrated sulfuric acid, remove surface coating layer;After deionized water is rinsed, then with speckling with absolute ethyl alcohol
Absorbent cotton repeatedly clean it is ensured that the coat of optical fiber surface is thoroughly got rid of;
(2) fbg removing overlay is put in glassware, add the agno of 0.1mol/l3Solution, addition guarantees to remove
The fbg of overlay is totally submerged, and instills 0.2mol/lnaoh solution to tan precipitate, then is added dropwise over 0.2mol/l ammonia
Water, side edged rocks glassware, till the sediment until generating is completely dissolved just;
(3) instilling mass concentration in glassware is 10% glucose solution, adds the volume of glucose solution to account for total solution
The 3%-5% of volume, and container is placed in 50-60 DEG C of water-bath heating, now, silverskin on fbg plated surface, but film is thick
Degree is relatively thin, and uniformity is not good;
(4) in the agno of 0.1mol/l3Add 0.2mol/l naoh solution until tan precipitate occurs in solution, more dropwise add
Enter 0.2mol/l ammoniacal liquor, side edged rocks glassware, till the sediment until generating is completely dissolved just, by it in ice bath
Middle cooling, then in temperature t=0 DEG C, adds the glucose solution accounting for cumulative volume 3%-8%, and its mass concentration is 12%, will
The fbg of the surface of step (3) gained plated film is immersed, and carries out second coating process, now it is observed that mixing
The color of thing from faint yellow, be changed into red, then be changed into grey, and the change of color represents and generates collargol and experience condensed
Journey, completes silver plating process.
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CN202402099U (en) * | 2011-12-31 | 2012-08-29 | 中国燃气涡轮研究院 | Oil-gas separator |
CN102830094A (en) * | 2012-08-30 | 2012-12-19 | 燕山大学 | Sapphire optical fiber probe sensor used for measuring gas holdup under oil well |
CN103512860A (en) * | 2012-06-19 | 2014-01-15 | 中南大学 | Method for monitoring dissolved gas in transformer oil based on terahertz wave photonic crystal fibers |
CN203551465U (en) * | 2013-11-06 | 2014-04-16 | 郑州光力科技股份有限公司 | On-line monitoring system for transformer oil |
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Publication number | Priority date | Publication date | Assignee | Title |
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WO1998050673A1 (en) * | 1997-05-09 | 1998-11-12 | Cidra Corporation | Packer having sensors for downhole inflation monitoring |
CN101126710A (en) * | 2007-09-13 | 2008-02-20 | 上海神开石油化工装备股份有限公司 | Drilling fluid gaseous hydrocarbon component quick non-disperse infrared spectrum determination method |
CN201083688Y (en) * | 2007-09-13 | 2008-07-09 | 上海神开石油化工装备股份有限公司 | Drilling fluid gaseous hydrocarbon component sensor |
CN101738382A (en) * | 2008-11-14 | 2010-06-16 | 香港理工大学 | Transformer failure gas monitoring system and method |
CN202402099U (en) * | 2011-12-31 | 2012-08-29 | 中国燃气涡轮研究院 | Oil-gas separator |
CN103512860A (en) * | 2012-06-19 | 2014-01-15 | 中南大学 | Method for monitoring dissolved gas in transformer oil based on terahertz wave photonic crystal fibers |
CN102830094A (en) * | 2012-08-30 | 2012-12-19 | 燕山大学 | Sapphire optical fiber probe sensor used for measuring gas holdup under oil well |
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