CN103293137A - Preparation method of optical fiber iron ion sensitive film - Google Patents
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 17
- 229920000447 polyanionic polymer Polymers 0.000 claims abstract description 13
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000033444 hydroxylation Effects 0.000 claims abstract description 9
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- -1 iron ion Chemical class 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
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- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 52
- 229910001447 ferric ion Inorganic materials 0.000 claims description 52
- 239000012528 membrane Substances 0.000 claims description 32
- 239000002243 precursor Substances 0.000 claims description 16
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims description 9
- 230000003068 static effect Effects 0.000 claims description 9
- GNKCWVPIWVNYKN-SFQUDFHCSA-N 5-[(e)-(3-carboxy-5-methyl-4-oxocyclohexa-2,5-dien-1-ylidene)-(2,6-dichloro-3-sulfophenyl)methyl]-2-hydroxy-3-methylbenzoic acid Chemical compound C1=C(C(O)=O)C(=O)C(C)=C\C1=C(C=1C(=C(C=CC=1Cl)S(O)(=O)=O)Cl)\C1=CC(C)=C(O)C(C(O)=O)=C1 GNKCWVPIWVNYKN-SFQUDFHCSA-N 0.000 claims description 6
- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 claims description 6
- 229940059939 kayexalate Drugs 0.000 claims description 6
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 claims description 5
- 230000008447 perception Effects 0.000 claims description 5
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 230000023077 detection of light stimulus Effects 0.000 claims description 4
- 239000001117 sulphuric acid Substances 0.000 claims description 4
- 235000011149 sulphuric acid Nutrition 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 3
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims description 2
- 238000005299 abrasion Methods 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 230000006870 function Effects 0.000 claims description 2
- 229920000083 poly(allylamine) Polymers 0.000 claims description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 2
- 230000001235 sensitizing effect Effects 0.000 claims description 2
- 229930192474 thiophene Natural products 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims 1
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- BHKKSKOHRFHHIN-MRVPVSSYSA-N 1-[[2-[(1R)-1-aminoethyl]-4-chlorophenyl]methyl]-2-sulfanylidene-5H-pyrrolo[3,2-d]pyrimidin-4-one Chemical compound N[C@H](C)C1=C(CN2C(NC(C3=C2C=CN3)=O)=S)C=CC(=C1)Cl BHKKSKOHRFHHIN-MRVPVSSYSA-N 0.000 abstract 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
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- 229910000838 Al alloy Inorganic materials 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
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- 241001251371 Betula chinensis Species 0.000 description 1
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- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention belongs to the technical field of optical fiber sensing and relates to a preparation method of an optical fiber iron ion sensitive film. The preparation method comprises the following steps of: firstly, carrying out preprocessing on the surface of an optical fiber or an optical grating to form an optical fiber or optical grating sensing region; secondly, successively immersing the optical fiber or optical grating sensing region into concentrated sulfuric acid/hydrogen peroxide solution and concentrated ammonia water/hydrogen peroxide solution to carry out hydroxylation preprocessing to hydroxylate the surface of the optical fiber or optical grating sensing region; and thirdly, alternatively immersing the hydroxylated optical fiber or optical grating sensing region into polyanion and polycation solution containing iron ion indicators, carrying out alternative preparation for 10-50 times by utilizing the conventional electrostatic self-assembly method, and drying by nitrogen, so as to prepare the optical fiber iron ion sensitive film. The preparation method has the advantages that the preparation process is simple, the principle is reliable, the prepared optical fiber iron ion sensitive film is controllable in thickness, and the online detection problem of iron ions which are early-stage corrosion products under concealed environments such as anticorrosive coatings can be solved.
Description
Technical field:
The invention belongs to technical field of optical fiber sensing, relate to preparation technology, particularly a kind of preparation method of optical fiber ferric ion sensitive membrane that a kind of optical fiber ferric ion detecting sensor is used sensitive membrane.
Background technology:
The seventies in 20th century, along with the development of optical fiber communication and photoelectron technology, occurring a kind of is transmission medium with the light wave, by the novel sensing technology of optical fiber perception and the extraneous measured signal of transmission, it is optical fiber sensing technology, the optical fiber volume is little, and quality is light, is convenient to be embedded in tested position and carries out in site measurement, and the working band of optical fiber is wide, dynamic range is big, is suitable for remote measuring and controlling, is a kind of excellent low loss transmission line; Optical fiber sensing technology has the characteristics of susceptibility height and anti-electromagnetic interference (EMI), can carry out the conversion of photoelectricity or electric light easily, easy and computer network is complementary and carries out the measurement of networking, has the incomparable advantage of other detection technique, be particularly suitable for using under the rugged surroundings such as inflammable, explosive, limited space and strong electromagnetic, utilize optical fiber sensing technology to detect hundreds of physichemical quantity, especially be fit to structure erosion monitoring and the health monitoring in hidden environment and non-contactable region territory.Optical fiber sensing technology began to detect research for the corrosion of facilities such as bridge and pipeline from the nineties, by the modulation of light wave parameter, can monitor iron and steel, aluminium alloy, aldary etc. corrosion and with the variation of the relevant environmental parameter (the pH value of solution, ambient humidity, temperature, corrosion product etc.) of corrosion; Detection by corrosion environment factor and corrosion product can be taked effective remedial measures in the early stage generation of just finding corrosion of corrosion before one-piece construction is damaged.Adopt optical fiber sensing technology more to the report of measurements such as pH value, ambient humidity and temperature at present, but the research that is used for the Fibre Optical Sensor that corrosion product detects is less, Chinese patent CN200510044326.5 detects the demand of copper ion at non-destructive in the corrosion of copper alloy process, discloses a kind of preparation method of the fiber-optic grating sensor that detects for copper ion; Liu Jianhuas etc. have reported that the aluminium ion that adopts fluorescence indicator to survey in the corrosion of aluminium alloy process changes; Bryant adopts synthetic ferric ion fluorescence probe that the corrosion of iron and steel under the coating is detected, and the technology that detects corrosion by ion probe has obtained good effect, but can not carry out online detection, can't be further used for corrosion monitoring system; Colourimetry or fluorescence method are generally adopted in the detection of ferric ion, are used for laboratory or on-the-spot offline inspection mostly, are not suitable for online detection; The upright equality of dragon has been reported a kind of preparation method who detects the ferric ion sensitive membrane, and contrasts with the test result of spectrophotometric method, has good consistance, and this method provides thinking for the research of carrying out optical fiber ferric ion detection technique.Now, the online detection of ferric ion is still a technical barrier, and existing ferric ion detection technique is combined with optical fiber sensing technology, seeks a kind of new solution, be expected to break through the limitation of prior art, form a kind of optical fiber ferric ion sensor that can carry out in situ detection.Optical fiber sensing corrosion monitoring technology development in recent years is rapid, especially the detection demand that is fit to hidden part and intelligence structure, this technology is at the early-stage in the application in oceanographic engineering field, but because the etching problem in oceanographic engineering field is outstanding relatively, the environment harshness, security to structure causes bigger threat, and existing optical fiber sensing corrosion monitoring technology has certain limitation in actual applications.
Summary of the invention:
The objective of the invention is to overcome the shortcoming that prior art exists, seek to design the preparation method that a kind of optical fiber ferric ion sensitive membrane is provided, technical barrier at the online detection of ferric ion, adopt optical fiber sensing technology, the sensitive membrane that has ferric ion susceptibility by the method for static self assembly in the optical fiber surface preparation, and then the optic response by sensitive membrane, realize the online detection of ferric ion Fibre Optical Sensor.
To achieve these goals, the present invention carries out pre-service to optical fiber or grating surface earlier, prepares the ferric ion sensitive membrane by the static self-assembling technique at optical fiber surface then, and its specific embodiment is:
(1), selects commercially available optical fiber or grating for use, earlier optical fiber or grating surface are carried out pre-service, adopting weight percent concentration is protective seam and the part covering that 10% HF acid etch or physics abrasion method are removed optical fiber or grating surface, and forming length at optical fiber or grating surface is optical fiber or the grating sensing zone of 1-6cm;
(2), optical fiber or grating sensing zone successively is immersed in strong aqua/hydrogen peroxide solution that the concentrated sulphuric acid/hydrogen peroxide solution that volume ratio is 7:3 and volume ratio be 1:1 at room temperature carries out hydroxylation pre-service 20-90 minute, make the surface hydroxylation in optical fiber or grating sensing zone;
(3), the ferric ion indicator is joined in polyanion precursor solution and the polycation precursor solution respectively, or join simultaneously in polyanion and the polycation precursor solution and to form polyanion and the polycation precursor solution that contains the ferric ion indicator, wherein, the weight percent concentration of ferric ion indicator is 0.1%-0.2%, the weight percent concentration of polyanion is 0.6%-0.8%, the weight percent concentration of polycation is 0.6%-0.8%;
(4), the optical fiber after the hydroxylation or grating sensitizing range alternately are immersed in the polyanion and polycation precursor solution that contains the ferric ion indicator, alternately prepare 10-50 time by existing static self-assembling method, employing nitrogen dries up, be prepared into optical fiber ferric ion sensitive membrane, the thickness of optical fiber ferric ion sensitive membrane is controlled by the number of times of alternately preparation.
The ferric ion indicator that the present invention relates to is the indicator with fluorescence or colour change function, comprises sulfosalicylic acid, phenanthroline, chrome azurol S and rhodamine; The polyanion precursor solution that relates to comprises kayexalate (PSS), poly-(3-carboxylic acid) thiophene (P3TEA) and polyacrylic acid (PAA); Polycation precursor solution comprises diallyl dimethyl ammoniumchloride (PDDA), polyene propyl group ammonium salt (PAn) and polyallylamine (PAH).
Iron concentration changes in the optical fiber ferric ion sensitive membrane energy perception solution of the present invention's preparation, when iron concentration changes, optical fiber ferric ion sensitive membrane is modulated the light signal that transmits in the optical fiber, can access the variable quantity of iron concentration by the detection of light signal.
The present invention and prior art, its preparation process is simple, principle is reliable, the optical fiber ferric ion sensitive membrane controllable thickness of preparation, can solve the problem on line detection of the early stage product ferric ion of corrosion under the hidden environment such as corrosion-inhibiting coating, the iron concentration that adopts the sensor of optical fiber ferric ion sensitive membrane preparation to can be used under the early detection of corroding under the hidden environment and circulation, the natural environmental condition detects, for the circulating water environmental monitoring of unifying provides online ferric ion detection method.
Embodiment:
Be further described below by the present invention of embodiment.
Embodiment 1:
Present embodiment adopts the preparation of static self-assembling method to have the ferric ion sensitive membrane at optical fiber surface, iron concentration changes in the ferric ion sensitive membrane energy perception solution of preparation, when iron concentration changes, sensitive membrane is modulated the light signal that transmits in the optical fiber, obtain the variable quantity of iron concentration by the detection of light signal, the concrete preparation process of ferric ion sensitive membrane is:
1. choose the ordinary optic fibre of a segment length 5-20cm, remove earlier the protective seam of optical fiber surface by physical method, adopting weight percent concentration then is that to form length at optical fiber surface be the Fibre Optical Sensor zone of 6cm for part covering that 10% HF acid etch method is removed optical fiber;
2. the Fibre Optical Sensor zone at room temperature successively is immersed in strong aqua/hydrogen peroxide solution that the concentrated sulphuric acid/hydrogen peroxide solution that volume ratio is 7:3 and volume ratio be 1:1 and carries out pre-service, pretreatment time is 20 minutes, obtains hydroxylated Fibre Optical Sensor zone;
3. hydroxylated Fibre Optical Sensor zone alternately is immersed in kayexalate (PSS) solution and diallyl dimethyl ammoniumchloride (PDDA) solution that contains ferric ion indicator sulfosalicylic acid, the weight percent concentration of sulfosalicylic acid is 0.2%, the weight percent concentration of kayexalate is 0.8%, the weight percent concentration of diallyl dimethyl ammoniumchloride is 0.8%, alternately prepare 20 times by the static self-assembling method, formation contains the self-assembled film of indicator sulfosalicylic acid, dry up with nitrogen then, namely obtain the ferric ion sensitive membrane.
Embodiment 2:
Present embodiment adopts the preparation of static self-assembling method to have the ferric ion sensitive membrane at grating surface, iron concentration changes in the ferric ion sensitive membrane energy perception solution of preparation, when iron concentration changes, sensitive membrane is modulated the light signal that transmits in the optical fiber, obtain the variable quantity of iron concentration by the detection of light signal, the concrete preparation process of ferric ion sensitive membrane is:
1. choose the long-period gratings that a segment length is 2-10cm, adopting weight percent concentration is that to form length be the grating sensing zone of 1cm for part covering that 10% HF acid etch method is removed grating surface;
2. the grating sensing zone at room temperature successively is immersed in strong aqua/hydrogen peroxide solution that the concentrated sulphuric acid/hydrogen peroxide solution that volume ratio is 7:3 and volume ratio be 1:1 and carries out pre-service, the processing time is 90 minutes, makes grating sensing area surfaces hydroxylation;
3. the Fibre Optical Sensor zone after the hydroxylation alternately is immersed in kayexalate (PSS) solution that contains ferric ion indicator chrome azurol S and contains in diallyl dimethyl ammoniumchloride (PDDA) solution of ferric ion indicator chrome azurol S, the weight percent concentration of chrome azurol S is 0.1%, the weight percent concentration of kayexalate is 0.6%, the weight percent concentration of diallyl dimethyl ammoniumchloride is 0.6%, method by the static self assembly alternately prepares 40 times, formation contains the self-assembled film of indicator chrome azurol S, dry up with nitrogen then, namely obtain the ferric ion sensitive membrane.
Claims (3)
1. the preparation method of an optical fiber ferric ion sensitive membrane is characterized in that earlier optical fiber or grating surface being carried out pre-service, prepares the ferric ion sensitive membrane by the static self-assembling technique at optical fiber surface then, and its specific embodiment is:
(1), selects commercially available optical fiber or grating for use, earlier optical fiber or grating surface are carried out pre-service, adopting weight percent concentration is protective seam and the part covering that 10% HF acid etch or physics abrasion method are removed optical fiber or grating surface, and forming length at optical fiber or grating surface is optical fiber or the grating sensing zone of 1-6cm;
(2), optical fiber or grating sensing zone successively is immersed in strong aqua/hydrogen peroxide solution that the concentrated sulphuric acid/hydrogen peroxide solution that volume ratio is 7:3 and volume ratio be 1:1 at room temperature carries out hydroxylation pre-service 20-90 minute, make the surface hydroxylation in optical fiber or grating sensing zone;
(3), the ferric ion indicator is joined in polyanion precursor solution and the polycation precursor solution respectively, or join simultaneously in polyanion and the polycation precursor solution and to form polyanion precursor solution and the polycation precursor solution that contains the ferric ion indicator, wherein, the weight percent concentration of ferric ion indicator is 0.1%-0.2%, the weight percent concentration of polyanion is 0.6%-0.8%, the weight percent concentration of polycation is 0.6%-0.8%;
(4), the optical fiber after step (2) hydroxylation or grating sensitizing range alternately are immersed in the polyanion precursor solution and polycation precursor solution that contains the ferric ion indicator, alternately prepare 10-50 time by existing static self-assembling method, employing nitrogen dries up, be prepared into optical fiber ferric ion sensitive membrane, the thickness of optical fiber ferric ion sensitive membrane is controlled by the number of times of alternately preparation.
2. the preparation method of optical fiber ferric ion sensitive membrane according to claim 1 is characterized in that the ferric ion indicator that relates to is the indicator with fluorescence or colour change function, comprises sulfosalicylic acid, phenanthroline, chrome azurol S and rhodamine; The polyanion precursor solution that relates to comprises kayexalate, poly-(3-carboxylic acid) thiophene and polyacrylic acid; Polycation precursor solution comprises diallyl dimethyl ammoniumchloride, polyene propyl group ammonium salt and polyallylamine.
3. the preparation method of optical fiber ferric ion sensitive membrane according to claim 1, iron concentration changes in the optical fiber ferric ion sensitive membrane energy perception solution that it is characterized in that preparing, when iron concentration changes, optical fiber ferric ion sensitive membrane is modulated the light signal that transmits in the optical fiber, can access the variable quantity of iron concentration by the detection of light signal.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107126847A (en) * | 2016-02-29 | 2017-09-05 | 中国石油化工股份有限公司 | Preparation method of a high-performance hollow fiber organic gas separation composite membrane |
| CN110806387A (en) * | 2019-11-12 | 2020-02-18 | 中国刑事警察学院 | Method for judging formation time of iron tannate ink handwriting |
| CN113418930A (en) * | 2021-06-04 | 2021-09-21 | 西北工业大学 | Method for rapidly detecting whether surface coating of iron plate is complete |
| CN116256333A (en) * | 2021-12-10 | 2023-06-13 | 山东省科学院生物研究所 | Method for improving sensitivity of LPFG detection on salt ion concentration |
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| CN107126847B (en) * | 2016-02-29 | 2020-02-18 | 中国石油化工股份有限公司 | A kind of preparation method of high-performance hollow fiber organic gas separation composite membrane |
| CN110806387A (en) * | 2019-11-12 | 2020-02-18 | 中国刑事警察学院 | Method for judging formation time of iron tannate ink handwriting |
| CN110806387B (en) * | 2019-11-12 | 2022-03-08 | 中国刑事警察学院 | Method for judging formation time of iron tannate ink handwriting |
| CN113418930A (en) * | 2021-06-04 | 2021-09-21 | 西北工业大学 | Method for rapidly detecting whether surface coating of iron plate is complete |
| CN113418930B (en) * | 2021-06-04 | 2024-05-10 | 西北工业大学 | Method for rapidly detecting whether surface coating of iron plate is complete |
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Application publication date: 20130911 |