CN100363768C - Process of preparing long period optical fiber raster for copper ion detecting - Google Patents
Process of preparing long period optical fiber raster for copper ion detecting Download PDFInfo
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- CN100363768C CN100363768C CNB2005100443265A CN200510044326A CN100363768C CN 100363768 C CN100363768 C CN 100363768C CN B2005100443265 A CNB2005100443265 A CN B2005100443265A CN 200510044326 A CN200510044326 A CN 200510044326A CN 100363768 C CN100363768 C CN 100363768C
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- Prior art keywords
- fiber grating
- optical fiber
- copper ion
- long period
- grating
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- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910001431 copper ion Inorganic materials 0.000 title claims abstract description 20
- 239000013307 optical fiber Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title abstract description 12
- 239000000835 fiber Substances 0.000 claims abstract description 45
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- 238000002444 silanisation Methods 0.000 claims abstract description 7
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 5
- 239000012190 activator Substances 0.000 claims abstract description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract 3
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract 3
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- RAABOESOVLLHRU-UHFFFAOYSA-N diazene Chemical compound N=N RAABOESOVLLHRU-UHFFFAOYSA-N 0.000 claims description 4
- 229910000071 diazene Inorganic materials 0.000 claims description 4
- -1 dimethylaminopropyl Chemical group 0.000 claims description 4
- 239000000017 hydrogel Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 125000001033 ether group Chemical group 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000012360 testing method Methods 0.000 abstract description 2
- 238000013098 chemical test method Methods 0.000 abstract 1
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 8
- 238000001514 detection method Methods 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 5
- 239000010949 copper Substances 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- 230000003595 spectral effect Effects 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052752 metalloid Inorganic materials 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 150000001455 metallic ions Chemical class 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- PXFBZOLANLWPMH-UHFFFAOYSA-N 16-Epiaffinine Natural products C1C(C2=CC=CC=C2N2)=C2C(=O)CC2C(=CC)CN(C)C1C2CO PXFBZOLANLWPMH-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000000246 remedial effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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Abstract
The invention relates to a manufacture method for copper ion testing using long cycle optical fiber grating in fiber sensing chemical testing technology field. It includes the following steps: adopting a normal optical fiber grating, removing oil stain on the surface by acetone, dipping in amine propyl 3-ethoxy silicane solution, drying in oven and making silanization, mixing carboxy activator with carboxymethyl cellulose water solution, putting the optical fiber grating into mixture liquid to take reaction to form optical fiber grating sensitive film on the surface, washing by distilled water and storing for use. The invention has simple process, reliable technology principle, and good savety.
Description
Technical field:
The invention belongs to the technology of preparing of a kind of fiber grating in the Fibre Optical Sensor chemical detection technique field, specifically a kind of preparation method of long period optical fiber raster for copper ion detecting.
Technical background:
Fibre Optical Sensor can detect various environmental parameters by different structural designs, such as water vapour, compound, stress, temperature and pressure etc.It is multiplexing that single Transmission Fibers cable can be finished multidata, and then carry out original position or remote recording monitoring.These performance advantages make Fibre Optical Sensor become the Perfected process of the corrosion monitoring of surveying hidden environment and non-contactable region territory.Technology at the non-destructive corrosion detective copper ion that uses aspect aviation, the naval vessel mainly contains EDDY CURRENT at present, ultrasound examination, dyestuff penetration and X-ray diffraction etc., but these methods are inapt to surveying early stage Corrosion results, usually because of the different differences to some extent of different testers' judgement.And these methods are difficult to distinguish reparation point and hot spot on the copper metalloid etching problem of determining sandwich construction.The key of corrosion detective is to realize the early stage measurement of corrosion, and preferably corrosion condition just can be detected out before the bulk strength of structure is destroyed, so just can take an effective remedial measures, and such reparation is only economy, actual.
The development of fiber grating has important promotion and influence to the development of optical fiber sensing technology.Fiber grating is the intrinsic facility of control light transmitting signal in the inside of optical fibre transmission, and they can be used as spectral filter, the scatter compensation element in the wavelength-division multiplex system etc.The sensitivity characteristic of grating is to be caused by the disturbance of ambient environmental conditions to optical fiber, thus fiber grating as the important component part of Fibre Optical Sensor and at the corrosive nature detection range especially to the detection range of copper metalloid corrosion condition by extensive studies and application.And employed fiber grating generally is made up of the optical fiber of periodic disturbance.The cycle General Definition of long-period gratings is that 100um is between the 1mm at wavelength.
Summary of the invention:
The objective of the invention is to seek a kind of being applied under the complex environment, metallic ion is the technology of preparation method of the long period fiber grating of copper ion detection usefulness particularly, and this method is by realizing the copper ion concentration in the monitoring solution after the sensitive membrane of long period fiber grating finishing macromolecular material.
In order to realize the foregoing invention purpose, after the finishing macromolecular material sensitive membrane of long period fiber grating, in order to the concentration of copper ion in the monitoring solution, detection signal is realized by the drift at spectrum spectrum peak.Purpose of the present invention realizes through the following steps:
(1) long period fiber grating is the grating structure that optical fiber surface formed, had the fixing cycle after treatment.Earlier fiber grating is cleaned to remove the greasy dirt on fiber grating surface with acetone;
(2) make solvent with ether or benzene respectively, the amine propyl-triethoxysilicane solution of preparation 1%-80%, long period fiber grating after cleaning was soaked 3-18 hour in amine propyl-triethoxysilicane solution, take out fiber grating and put into to dry under the baking oven 10-30 ℃ condition and make the fiber grating silanization;
(3) 1-ethyl-3-(3-dimethylaminopropyl)-carbon diimide (EDAC) aqueous solution of preparation 5-175mg/ml;
(4) utilize the EDAC aqueous solution to do carboxyl activator, with carboxymethyl cellulose (CMC) aqueous solution of 10%-80%, the fiber grating of silanization is put in the above-mentioned mixed liquor and reacted 1-5 hour.By this course of reaction, on fiber grating, made a kind of crosslinked hydrogel and constituted the fiber grating sensitive membrane as fiber-optic grating sensor, its stable performance is used for detecting the concentration of solution copper ion;
(5) clean up and be stored in the distilled water fiber grating sensitive membrane stand-by with distilled water at last.
The inventive method preparation is used to detect the long period fiber grating of copper ion concentration, and its preparation process is simple, and the technology principle is reliable, its product is used for detecting the copper ion concentration of the copper metalloid corrosion occasion under the rugged surroundings, its measuring method is convenient, and data are reliable, handling safety.
Description of drawings:
Fig. 1 is for forming the optical fiber grating structure principle schematic of crosslinked hydrogel.
Fig. 2 detects the spectral strength of copper ion concentration with concentration curve figure.
Fig. 3 is for detecting the spectrogram of variable concentrations copper ion.
Embodiment:
Fiber grating is the grating structure that fixed cycle is arranged with the optical means etching on the fibre core surface.It is responsive more to the variation of surrounding environment parameter.By in the outside modified macromolecule material sensitive membrane of its covering, reach the purpose that detects metallic ion.When this rete runs into copper ion in the solution, adsorption volume taking place expand, makes the refractive index of covering change.According to the A of publicity: λ=(ncore-nclad), wherein λ represents the centre wavelength of grating, and ncore and nclad represent the refractive index of fibre core and covering respectively, and Λ represents the grating cycle.The variation of cladding index causes the drift of grating centre wavelength and the variation of spectral energy.
Embodiment:
The structure of the long period fiber grating that the invention process is finished is formed and is comprised grating 1, covering 2, fibre core 3, affine coating 4 and sensitive membrane 5; The main body of fiber grating is selected commercially available finished product for use, forms sensitive membrane 5 through the present invention.
Get a fiber grating, length is about 40 centimetres, 2 centimetres of grating lengths, clean grating after 10 minutes with acetone earlier, put into ether do solvent, concentration is that 50% amine propyl-triethoxysilicane soaked 4 hours, take out the back and in conventional baking oven, dry under 20 ℃ of conditions, and make the fiber grating silanization;
1-ethyl-3-(3-dimethylaminopropyl)-carbon diimide (EDAC) aqueous solution of preparation 35mg/ml is done carboxyl activator, carboxymethyl cellulose (CMC) aqueous solution with 10%, the fiber grating of silanization is put in above-mentioned mixed liquor reaction 1 hour, on the fiber grating surface, made a kind of crosslinked hydrogel sensitive membrane, its stable performance is used for detecting the concentration of solution copper ion.
The fiber grating that this process preparation forms as a kind of susceptibility preferably fiber-optic grating sensor owing to be that reaction forms in mixed liquor, take out and to use distilled water flushing after the mixed liquor totally guaranteeing that it does not leave over mixed liquor, but and long-term storage stand-by in distilled water.
Utilize spectrometer detect above-mentioned fiber grating in different Cu ion concentration solution spectral strength and the situation of change of centre wavelength, testing result can be shown by curve map and spectrogram, its presentation of results has good sensitivity as sensor to the concentration of copper ion with the fiber grating sensitive membrane of method for preparing, can carry out the detection of copper ion concentration.
Claims (3)
1. the preparation method of a long period optical fiber raster for copper ion detecting, it is characterized in that earlier fiber grating being cleaned with acetone removing its surperficial greasy dirt, place it in again to soak in the amine propyl-triethoxysilicane solution and put into after 3-18 hour that oven dry makes the fiber grating silanization under the baking oven 10-30 ℃ condition; Do carboxyl activator with 1-ethyl-3-(3-dimethylaminopropyl)-carbon diimide aqueous solution, carboxymethyl cellulose aqueous solution with 10% mixes, the fiber grating of silanization was put in the mixed liquor reaction 1-5 hour, on fiber grating, make crosslinked hydrogel and constitute the fiber grating sensitive membrane, clean up and be stored in the distilled water fiber grating sensitive membrane stand-by with distilled water.
2. the preparation method of long period optical fiber raster for copper ion detecting according to claim 1 is characterized in that used fiber grating length is 40 centimetres, and grating length is 2 centimetres; The time of cleaning with acetone is 10 minutes; Amine propyl-triethoxysilicane solution concentration is 50%, and its solvent is ether or benzene.
3. the preparation method of long period optical fiber raster for copper ion detecting according to claim 1,1-ethyl-3-(3-the dimethylaminopropyl)-carbon diimide aqueous solution that it is characterized in that preparing 35mg/ml is mixed with carboxymethyl cellulose aqueous solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100443265A CN100363768C (en) | 2005-07-29 | 2005-07-29 | Process of preparing long period optical fiber raster for copper ion detecting |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100443265A CN100363768C (en) | 2005-07-29 | 2005-07-29 | Process of preparing long period optical fiber raster for copper ion detecting |
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| Publication Number | Publication Date |
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| CN1904657A CN1904657A (en) | 2007-01-31 |
| CN100363768C true CN100363768C (en) | 2008-01-23 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103293137A (en) * | 2013-06-08 | 2013-09-11 | 中国船舶重工集团公司第七二五研究所 | Preparation method of optical fiber iron ion sensitive film |
| CN103941330A (en) * | 2014-05-07 | 2014-07-23 | 南通大学 | Composite structure long-period fiber grating |
| CN107907474A (en) * | 2017-11-20 | 2018-04-13 | 江苏科技大学 | A kind of novel sensor and its manufacture method and implementation |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5633748A (en) * | 1996-03-05 | 1997-05-27 | The United States Of America As Represented By The Secretary Of The Navy | Fiber optic Bragg grating demodulator and sensor incorporating same |
| US5646400A (en) * | 1995-07-14 | 1997-07-08 | The United States Of America As Represented By The Secretary Of The Navy | Corrosion detecting and monitoring method and apparatus |
| CN1166872A (en) * | 1994-11-29 | 1997-12-03 | 联合技术公司 | Optical fiber bragg grating coating removal detection |
| CN1167527A (en) * | 1994-11-29 | 1997-12-10 | 联合技术公司 | Highly sensitive optical fiber cavity coating removal detection |
| US6144026A (en) * | 1997-10-17 | 2000-11-07 | Blue Road Research | Fiber optic grating corrosion and chemical sensor |
| CN2567548Y (en) * | 2002-09-13 | 2003-08-20 | 西安石油学院 | Fibre-optical grating sensor for testing gas-oil pipe |
-
2005
- 2005-07-29 CN CNB2005100443265A patent/CN100363768C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1166872A (en) * | 1994-11-29 | 1997-12-03 | 联合技术公司 | Optical fiber bragg grating coating removal detection |
| CN1167527A (en) * | 1994-11-29 | 1997-12-10 | 联合技术公司 | Highly sensitive optical fiber cavity coating removal detection |
| US5646400A (en) * | 1995-07-14 | 1997-07-08 | The United States Of America As Represented By The Secretary Of The Navy | Corrosion detecting and monitoring method and apparatus |
| US5633748A (en) * | 1996-03-05 | 1997-05-27 | The United States Of America As Represented By The Secretary Of The Navy | Fiber optic Bragg grating demodulator and sensor incorporating same |
| US6144026A (en) * | 1997-10-17 | 2000-11-07 | Blue Road Research | Fiber optic grating corrosion and chemical sensor |
| CN2567548Y (en) * | 2002-09-13 | 2003-08-20 | 西安石油学院 | Fibre-optical grating sensor for testing gas-oil pipe |
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| CN1904657A (en) | 2007-01-31 |
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