CN104359859A - Method for improving refractive index detecting sensitivity of long period fiber gratings - Google Patents
Method for improving refractive index detecting sensitivity of long period fiber gratings Download PDFInfo
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- CN104359859A CN104359859A CN201410715985.6A CN201410715985A CN104359859A CN 104359859 A CN104359859 A CN 104359859A CN 201410715985 A CN201410715985 A CN 201410715985A CN 104359859 A CN104359859 A CN 104359859A
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Abstract
The invention discloses a method for improving the refractive index detecting sensitivity of long period fiber gratings. The detecting sensitivity is improved by quickly and controllably preparing zirconium dioxide or tantalum pentoxide nano films in proper thickness on the surfaces of the long period fiber gratings through liquid deposition. The method has the advantages that expensive instruments and equipment are not needed; the operation process is simple and convenient; the time spent on regulating the sensitivity of the long period fiber gratings is saved; the refractive index regulation efficiency of the long period fiber gratings is improved; the cost needed for manufacturing long period fiber grating sensors with high sensitivity is reduced.
Description
Technical field
The present invention relates to long period fiber grating detection technique field, particularly relate to a kind of method improving the sensitivity of detection long period fiber grating refractive index.
Background technology
Refractive index is the important parameter characterizing material optical property, the purity, concentration etc. of its optical property, material can be understood by the refractive index studying material, therefore study, predict and design the senser element of the refractive index that can induce particular demands, for exploitation new optical material and there is important Research Significance in the application of optical field, for realizing its application at numerous areas such as commercial production, environmental monitoring, food inspection, clinical examination, drug screening, metallurgy, also there is important research value.
Long period fiber grating is a kind of passive optical senser element ambient refractive index to sensitive property, attempted being used for the measurement of liquid refractivity, as " photoelectric technology application " 2008.23(4) deliver the Shandong beautiful spring-time, letter is aquatic to be waited " index sensor based on long period fiber grating " collaborateed, " Sensors and Actuators B " 2001.74:74 has delivered R. Falciai, A.G. Mignani, A. Vannini collaborate " Long period gratings as solution concentration sensors ", " Optics Communications " 2004.229:65 has delivered Joo Hin Chong, " Measurements of refractive index sensitivity using long-period grating refractometer " that Ping Shum etc. collaborate.Their result of study proves, long-period gratings refractive index has higher sensitivity.
But, as the Sarfraz Khaliq that " Measurement Science and Technology " 2002. 13:792 deliver, Stephen W James, described in " Enhanced sensitivity fibre optic long period grating temperature sensor " literary composition that Ralph P Tatam collaborates, general naked long-period gratings is only sensitiveer to the ambient refractive index in 1.400 ~ 1.456 scopes, and is low-down to the sensitivity of aqueous solution (refractive index 1.333) or gas medium.The refractive index being detected surrounding medium due to majority is between 1.0-1.4, and this is totally unfavorable to the application in practice of exploitation long period fiber grating.
Along with the develop rapidly of nano material and nanometer-material-modified technology, for the response sensitivity explored and change long-period grating pair ambient refractive index provides brand-new approach, scientific research personnel has carried out much relevant research.Some achievements in research show, when the nano thin-film coating high at long-period gratings surface deposition refractive index ratio grating covering, the sensitive property of long-period gratings to ambient refractive index is increased significantly, as " Optics Express " 2005,13(1): 56 have delivered Ignacio Del Villar, Ignacio R. Mat í as, " Optimization of sensitivity in Long Period Fiber Gratings with overlay deposition " that Francisco J. Arregui collaborates, " Reactive and Functional Polymers " 2011,71 (3): 335 have delivered Li Qiu-shun, " Enhanced sucrose sensing sensitivity of long period fiber grating by self-assembled polyelectrolyte multilayers " that Zhang Xu-lin etc. collaborate, " Optics Communications " 2014,331:39 has delivered Qiu-Shun Li, " Improved detecting sensitivity of long period fiber gratings by polyelectrolyte multilayers:The effect of film structures " that Xu-Lin Zhang etc. collaborate.They utilize electrostatic layer-by-layer to regulate and control the thickness of long-period gratings nano surface film, and regulation and control long-period gratings, makes it respectively to the sensitivity that the surrounding material of different refractivity is put up the best performance.
Electrostatic layer-by-layer is the electrostatic interaction between a kind of material utilizing oppositely charged, the technology of multi-layer ultrathin membrane is formed at substrate surface alternating deposit, compared with other numerous nano thin-film preparation method, this self-assembling technique has many good qualities, as: (1) method for manufacturing thin film is easy, only need immerse in solution by substrate, static a period of time, whole process does not need instrument and equipment and the operating environment of complex and expensive, can operate under room temperature condition; (2) by regulating the parameter of solution as the ionic strength, pH, concentration, ionic species etc. of solution, from the thickness of controlling diaphragm molecular level, structures and characteristics, can provide convenience for preparing optical functional film on long-period gratings surface.
But its unfavorable factor existed is, this technology is very consuming time, because the thickness of usual every one deck is only a few nanometer or tens nanometers, and be in best susceptibility to adjust long-period gratings to detecting medium, usually will assemble tens layers or hundreds of layers of nano thin-film at grating surface, this spends the time of a couple of days to complete with regard to needing.And under strong acid or strong base solution condition, this film is very easily destroyed to be dissociated or is out of shape, and stability is very poor.
Also there are some bibliographical informations, by the method for the solution (as the organic solvent solution of high molecular polymer or the sol gel solution of metal oxide) of direct dip-coating high index of refraction material, directly prepare nano thin-film rapidly on long-period gratings surface.Although this method can realize the thickness increasing nano thin-film quickly, adjust long-period gratings quickly to the sensitivity of ambient refractive index, but this method is difficult to the thickness accurately controlling film, is difficult to the sensitivity accurately regulating and controlling long-period gratings.
Overcome or eliminate these shortcomings that electrostatic LBL self-assembly, directly dip coating exist, the film-forming method of new adjustment long-period gratings sensitivity must be found.
Summary of the invention
Object of the present invention is exactly defect for above-mentioned existence and provides a kind of and improve the method detecting the sensitivity of long period fiber grating refractive index.
A kind of method and technology scheme detecting the sensitivity of long period fiber grating refractive index that improves of the present invention is, by the method for liquid deposition at long-period gratings surface deposition zirconium dioxide or tantalum pentoxide nano thin-film.
After stretching for long period fiber grating fixing, be added in the liquid of grating surface growth zirconium dioxide or tantalum pentoxide nano thin-film, by controlling time and the temperature of the kind of reaction reagent in reaction solution, concentration and reaction solution, control the thickness of zirconium dioxide or tantalum pentoxide nano thin-film, the sensitive range of quick regulation and control long-period grating pair ambient refractive index, thus improve the sensitivity of detection long period fiber grating refractive index.
A kind of described method improving the sensitivity of detection long period fiber grating refractive index, specifically comprises the following steps:
The solution of (a) preparation growth zirconium dioxide or tantalum pentoxide nano thin-film;
B () is stretching fixing on the stationary fixture support containing reactive tank by long period fiber grating;
C cleaning process is carried out in the grid region substrate of () long period fiber grating;
D () joins the solution of the growth zirconium dioxide prepared or tantalum pentoxide nano thin-film and fixes in the reactive tank of long-period gratings;
E (), to the heating liquid in reactive tank, controls temperature of reaction, zirconium dioxide or tantalum pentoxide nano thin-film are increased on long-period gratings surface;
F () controls the time of reaction, the growth thickness of zirconium dioxide or tantalum pentoxide nano thin-film is controlled with this, and then adjustment long-period gratings is to the sensitive range of different refractivity, stop reaction when the sensitivity of long-period gratings refractive index reaches necessary requirement;
G () has the long-period gratings of zirconium dioxide or tantalum pentoxide nano thin-film to rinse with redistilled water to growth, remove unreacted liquid and impurity.
In step (a), the solution of growth Zirconium dioxide nano thin film comprises the one in zirconium sulfate, sodium fluozirconate or hexafluoro zirconate solution; The solution of growth tantalum pentoxide nano thin-film comprises ethanol tantalum solution.
The concentration of aqueous solution of ethanol tantalum, zirconium sulfate, sodium fluozirconate or hexafluoro zirconate is 0.0001 ~ 10 mol/L.
When grow the solution of Zirconium dioxide nano thin film to be made up of sodium fluozirconate and boric acid or hexafluoro zirconate and boric acid form time, the mol ratio of sodium fluozirconate and boric acid or hexafluoro zirconate and boric acid is 1:0.5 ~ 50; When grow the solution of Zirconium dioxide nano thin film to be made up of sodium fluozirconate and metallic aluminium or hexafluoro zirconate and metallic aluminium form time, the mol ratio of sodium fluozirconate and metallic aluminium or hexafluoro zirconate and metallic aluminium is 1:0.05 ~ 100; When the solution growing Zirconium dioxide nano thin film is made up of zirconium sulfate and ammonium persulfate, the mol ratio of zirconium sulfate and ammonium persulfate is 1:0.001 ~ 100; When the solution growing Zirconium dioxide nano thin film is made up of zirconium sulfate and hydrochloric acid, the mol ratio of zirconium sulfate, HCl is 1:0.001 ~ 2000.
Step (c) is specially: with volume ratio to be the concentrated sulphuric acid of 7:3 and mass concentration be 30% the washing lotion that forms of hydrogen peroxide cleaning carried out to the substrate of long period fiber grating grid region process.
In step (e), range of reaction temperature is 20 ~ 180 DEG C.
Zirconium dioxide or tantalum pentoxide nano thin-film is prepared, at least one nano particle in film in all right doping stannic oxide, zinc paste, indium oxide, titania, di-iron trioxide, tri-iron tetroxide, silicon dioxide, gold, silver, platinum, cadmium sulfide, zinc sulphide, cadmium telluride, indium phosphide, lead selenide, vulcanized lead, silicon quantum dot and carbon quantum dot at long-period gratings grid region cladding surface.
Prepare zirconium dioxide or tantalum pentoxide nano thin-film at long-period gratings grid region cladding surface, at zirconium dioxide or tantalum pentoxide nano thin-film surface fixed function identification material, can also can carry out specific recognition for biochemical molecular.
Beneficial effect of the present invention is: the present invention controllably prepares zirconium dioxide or the tantalum pentoxide nano thin-film of suitable thickness fast on long period fiber grating surface by liquid deposition, improve detection sensitivity.Concrete grammar is: after stretching for long period fiber grating fixing, add the liquid that can grow zirconium dioxide or tantalum pentoxide nano thin-film at grating surface, by controlling time and the temperature of the kind of reaction reagent in reaction solution, concentration and reaction solution, control the thickness of nano thin-film, the sensitive range of quick regulation and control long-period grating pair ambient refractive index, thus regulate and control the sensitivity of long period fiber grating rapidly.Specifically there is following advantage:
(1) the inventive method, simple to operate, do not need the specific installations such as high temperature, vacuum, high frequency, high pressure, can complete under atmospheric pressure environment.
(2) the inventive method, the raw material used is easy to get, and can be according to actual needs, on nanoscale, directly regulate the speed of growth of long period fiber grating surface film rapidly and accurately, regulate the thickness of nano thin-film rapidly and accurately, adjust the sensitive range of long-period grating pair different refractivity rapidly and accurately.
(3) the inventive method, compared with electrostatic layer by layer self-assembling method, the coating process of adjustment long period fiber grating sensitivity generally can complete in several hours, greatly save the masking time (shortening to several hours or dozens of minutes in tens hours hundreds of hours from LBL self-assembly nanometer technology), greatly increase the efficiency of regulation and control long period fiber grating sensitivity.
(4) the inventive method, compared with electrostatic layer by layer self-assembling method, obtained nano thin-film stability is stronger, is not subject to the impact of the conditions such as soda acid, ionic strength, buffer concentration, advantageously in the detection to biochemical substances.
(5) the inventive method, compared with the method for the solution of direct dip-coating high index of refraction material, more accurately can control the thickness of nano thin-film, more accurately regulates and controls long-period gratings to the sensitivity of ambient refractive index.
(6) the inventive method, the zirconium dioxide used or tantalum pentoxide nano thin-film have stronger acid-alkali-corrosive-resisting performance, and chemical stability is better.
(7) the inventive method, the zirconium dioxide used or tantalum pentoxide nano thin-film have good optical property and the good biocompatibilities such as high refraction, low dispersion, low-loss, are very suitable for the detection of further biochemical molecular.
accompanying drawing illustrates:
Figure 1 shows that long-period gratings is fixed and reaction unit diagrammatic cross-section.
In figure: 1, long-period gratings stationary installation, 2, reactive tank, 3, long period fiber grating, 4, reaction solution, 5, stationary installation screw.
embodiment:
In order to understand the present invention better, describe technical scheme of the present invention in detail with instantiation below.
After stretching for long period fiber grating 3 fixing, the reaction solution 4 that can grow zirconium dioxide or tantalum pentoxide nano thin-film nano thin-film at grating surface is added in the reactive tank 2 of long-period gratings stationary installation 1, by controlling time and the temperature of the kind of reaction reagent in reaction solution, concentration and reaction solution, control the thickness of zirconium dioxide or tantalum pentoxide nano thin-film, the sensitive range of quick regulation and control long period fiber grating 3 pairs of ambient refractive index, thus the sensitivity regulating and controlling long period fiber grating 3 rapidly.As shown in Figure of description Fig. 1, wherein, long period fiber grating 3 is fixed by stationary installation screw 5.
Embodiment 1
Ethanol tantalum dissolved in ethanol and fully stirs, being made into the ethanolic solution of 0.5ml 3.85mol/L ethanol tantalum, temperature being cooled to 10 DEG C, then add the ethanol water that 20ml mass ratio is 95%, and fully stir, then be cooled to 10 DEG C.Joined mixed liquor is poured into the reactive tank 2 of long-period gratings stationary installation 1, temperature of reaction is controlled at 10 DEG C, reaction is stopped when reaching 30min when reacted, and rinse 6 times with redistilled water, the now refractive index sensitivity of long period fiber grating 3 pairs of ethanol reaches 3100nm/RIU, improves 50 times than sensitivity when not growing tantalum pentoxide nano thin-film.
Embodiment 2
Prepare aqueous solution and the 30ml0.01mol/L boron aqueous acid of 10ml0.01mol/L sodium fluozirconate respectively, then 0.01mol/L boron aqueous acid is dropwise added drop-wise in the aqueous solution of 0.01mol/L sodium fluozirconate, subsequently mixed solution is fully stirred, joined mixed liquor is poured into the reactive tank 2 of long-period gratings stationary installation 1, the temperature of reaction solution is transferred to 60 DEG C, reaction is stopped when controlling 70 minutes reaction time, and fully rinse with redistilled water, the now refractive index sensitivity of long period fiber grating 3 pairs of normal butyl alcohols reaches 3700nm/RIU, improve 126 times than sensitivity when not growing Zirconium dioxide nano thin film.
Embodiment 3
Prepare the aqueous solution of 20ml0.01mol/L zirconium sulfate and the aqueous solution of 40ml0.01mol/L ammonium persulfate respectively, then by two kinds of Solutions Solution, and fully stirring makes it to mix, joined mixed liquor is poured into the reactive tank 2 of long-period gratings stationary installation 1, the temperature of reaction solution is transferred to 50 DEG C, reaction is stopped when being 40 minutes when reacted, and fully rinse with redistilled water, the now refractive index sensitivity of long period fiber grating 3 pairs of isopropyl alcohols reaches 2110nm/RIU, improves 43 times than sensitivity when not growing Zirconium dioxide nano thin film.
Embodiment 4
Prepare aqueous solution and the 20ml0.8M hydrochloric acid solution of 20ml8mM zirconium sulfate respectively, then by two kinds of Solutions Solution, and fully stirring makes it to mix, joined mixed liquor is poured into the reactive tank 2 of long-period gratings stationary installation 1, the temperature of reaction solution is transferred to 90 DEG C, reaction is stopped when being 90 minutes when reacted, and fully rinse with redistilled water, the now refractive index sensitivity of long period fiber grating 3 pairs of water reaches 1480nm/RIU, improves 19 times than sensitivity when not growing Zirconium dioxide nano thin film.
Embodiment 5
The aqueous solution of preparation 40ml0.06mol/L hexafluoro zirconate, abundant stirring, then solution is poured into the reactive tank 2 of long-period gratings stationary installation 1,15 grams of metallic aluminium particles are added subsequently to reactive tank 2, the temperature of reaction solution is transferred to 30 DEG C, stops reaction when controlling 55 minutes reaction time, and fully rinse with redistilled water, the now refractive index sensitivity of long period fiber grating 3 pairs of air reaches 1890nm/RIU, improves 66 times than sensitivity when not growing Zirconium dioxide nano thin film.
Claims (10)
1. improve the method detecting the sensitivity of long period fiber grating refractive index, it is characterized in that, by the method for liquid deposition at long-period gratings surface deposition zirconium dioxide or tantalum pentoxide nano thin-film.
2. a kind of method improving the sensitivity of detection long period fiber grating refractive index according to claim 1, it is characterized in that, after stretching for long period fiber grating fixing, be added in the liquid of grating surface growth zirconium dioxide or tantalum pentoxide nano thin-film, by controlling the kind of reaction reagent in reaction solution, the time of concentration and reaction solution and temperature, control the thickness of zirconium dioxide or tantalum pentoxide nano thin-film, the sensitive range of quick regulation and control long-period grating pair ambient refractive index, thus improve the sensitivity of detection long period fiber grating refractive index.
3. a kind of method improving the sensitivity of detection long period fiber grating refractive index according to claim 1, is characterized in that, comprise the following steps:
The solution of (a) preparation growth zirconium dioxide or tantalum pentoxide nano thin-film;
B () is stretching fixing on the stationary fixture support containing reactive tank by long period fiber grating;
C cleaning process is carried out in the grid region substrate of () long period fiber grating;
D () joins the solution of the growth zirconium dioxide prepared or tantalum pentoxide nano thin-film and fixes in the reactive tank of long-period gratings;
E (), to the solution heating in reactive tank, controls temperature of reaction, zirconium dioxide or tantalum pentoxide nano thin-film are increased on long-period gratings surface;
F () controls the time of reaction, the growth thickness of zirconium dioxide or tantalum pentoxide nano thin-film is controlled with this, and then adjustment long-period gratings is to the sensitive range of different refractivity, stop reaction when the sensitivity of long-period gratings refractive index reaches necessary requirement;
G () has the long-period gratings of zirconium dioxide or tantalum pentoxide nano thin-film to rinse with redistilled water to growth, remove unreacted liquid and impurity.
4. a kind of method improving the sensitivity of detection long period fiber grating refractive index according to claim 3, it is characterized in that, in step (a), the solution of growth Zirconium dioxide nano thin film comprises the one in zirconium sulfate, sodium fluozirconate or hexafluoro zirconate solution; The solution of growth tantalum pentoxide nano thin-film comprises ethanol tantalum solution.
5. a kind of method improving the sensitivity of detection long period fiber grating refractive index according to claim 4, is characterized in that: the concentration of aqueous solution of ethanol tantalum, zirconium sulfate, sodium fluozirconate or hexafluoro zirconate is 0.0001 ~ 10 mol/L.
6. a kind of method improving the sensitivity of detection long period fiber grating refractive index according to claim 5, it is characterized in that, when grow the solution of Zirconium dioxide nano thin film to be made up of sodium fluozirconate and boric acid or hexafluoro zirconate and boric acid form time, the mol ratio of sodium fluozirconate and boric acid or hexafluoro zirconate and boric acid is 1:0.5 ~ 50; When grow the solution of Zirconium dioxide nano thin film to be made up of sodium fluozirconate and metallic aluminium or hexafluoro zirconate and metallic aluminium form time, the mol ratio of sodium fluozirconate and metallic aluminium or hexafluoro zirconate and metallic aluminium is 1:0.05 ~ 100; When the solution growing Zirconium dioxide nano thin film is made up of zirconium sulfate and ammonium persulfate, the mol ratio of zirconium sulfate and ammonium persulfate is 1:0.001 ~ 100; When the solution growing Zirconium dioxide nano thin film is made up of zirconium sulfate and hydrochloric acid, the mol ratio of zirconium sulfate, HCl is 1:0.001 ~ 2000.
7. a kind of method improving the sensitivity of detection long period fiber grating refractive index according to claim 3, it is characterized in that, step (c) is specially: with volume ratio to be the concentrated sulphuric acid of 7:3 and mass concentration be 30% the washing lotion that forms of hydrogen peroxide cleaning carried out to the substrate of long period fiber grating grid region process.
8. a kind of method improving the sensitivity of detection long period fiber grating refractive index according to claim 3, is characterized in that: controlling range of reaction temperature in step (e) is 20 ~ 180 DEG C.
9. a kind of method improving the sensitivity of detection long period fiber grating refractive index according to claim 1, it is characterized in that, zirconium dioxide or tantalum pentoxide nano thin-film is prepared, at least one nano particle in film in doping stannic oxide, zinc paste, indium oxide, titania, di-iron trioxide, tri-iron tetroxide, silicon dioxide, gold, silver, platinum, cadmium sulfide, zinc sulphide, cadmium telluride, indium phosphide, lead selenide, vulcanized lead, silicon quantum dot and carbon quantum dot at long-period gratings grid region cladding surface.
10. a kind of method improving the sensitivity of detection long period fiber grating refractive index according to claim 1, it is characterized in that, zirconium dioxide or tantalum pentoxide nano thin-film is prepared, at zirconium dioxide or tantalum pentoxide nano thin-film surface fixed function identification material at long-period gratings grid region cladding surface.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109709074A (en) * | 2019-01-21 | 2019-05-03 | 哈尔滨理工大学 | Optical fiber ammonia gas sensor and production method based on Ag doping zinc oxide nanometer flower |
| CN112711090A (en) * | 2020-12-17 | 2021-04-27 | 山东省科学院生物研究所 | Method for regulating LPFG sensitivity by polymethacrylic acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109709074A (en) * | 2019-01-21 | 2019-05-03 | 哈尔滨理工大学 | Optical fiber ammonia gas sensor and production method based on Ag doping zinc oxide nanometer flower |
| CN112711090A (en) * | 2020-12-17 | 2021-04-27 | 山东省科学院生物研究所 | Method for regulating LPFG sensitivity by polymethacrylic acid |
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