CN104359858A - Method for quickly regulating refractive index sensitivity of long period fiber gratings - Google Patents
Method for quickly regulating refractive index sensitivity of long period fiber gratings Download PDFInfo
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- CN104359858A CN104359858A CN201410715982.2A CN201410715982A CN104359858A CN 104359858 A CN104359858 A CN 104359858A CN 201410715982 A CN201410715982 A CN 201410715982A CN 104359858 A CN104359858 A CN 104359858A
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Abstract
The invention discloses a method for quickly regulating the refractive index sensitivity of long period fiber gratings. The detecting sensitivity is improved by quickly and controllably preparing titanium dioxide 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 the method for a kind of quick regulation and control long period fiber grating refractive index sensitivity.
Background technology
Refractive index is one of important optical parametric of reflection material essence.By the measurement of refractive index, the optical property of solution and the much character such as purity, concentration, biochemical reaction parameter of material can be understood, therefore the measurement of refractive index has important Research Significance and using value widely at numerous areas such as commercial production, environmental monitoring, food inspection, clinical examination, drug screening, metallurgy and scientific researches, and the research of refractive index detection method and device also attracts widespread attention more and more.
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 and direct 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 the method for a kind of quick regulation and control long period fiber grating refractive index sensitivity.
The method and technology scheme of a kind of quick regulation and control long period fiber grating refractive index of the present invention sensitivity is, by the method for liquid deposition at long-period gratings surface deposition titanium dioxide nano-film.
After stretching for long period fiber grating fixing, be added in the liquid of grating surface growth titanium dioxide nano-film, by controlling time and the temperature of the kind of reaction reagent in reaction solution, concentration and reaction solution, control the thickness of titanium dioxide nano-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.
The method of described a kind of quick regulation and control long period fiber grating refractive index sensitivity, specifically comprises the following steps:
The solution of (a) preparation growth titanium dioxide nano-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 titanium dioxide nano-film prepared and fixes in the reactive tank of long-period gratings;
E (), to the solution heating in reactive tank, controls temperature of reaction, titanium dioxide nano-film is increased on long-period gratings surface;
F () controls the time of reaction, control the growth thickness of titanium dioxide nano-film with this, and then adjustment long-period gratings is to the sensitive range of different refractivity, stops reaction when the sensitivity of long-period gratings refractive index reaches necessary requirement;
G () has the long-period gratings of titanium dioxide nano-film to rinse with redistilled water to growth, remove unreacted liquid and impurity.
The solution of preparation growth titanium dioxide nano-film is at least one in titanium tetrafluoride, titanium tetrachloride, titanyl sulfate or the mixed solution for ammonium hexa-fluorotitanate and boric acid in step (a).
The concentration of aqueous solution of titanium tetrafluoride, titanium tetrachloride, titanyl sulfate or ammonium hexa-fluorotitanate is 0.0001 ~ 10 mol/L.
In step (a), when reactant liquor is made up of ammonium hexa-fluorotitanate and boric acid, ammonium hexa-fluorotitanate, boric acid mol ratio are 1:0.5 ~ 50.
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.
In long-period gratings grid region, cladding surface prepares titanium dioxide nano-film, at least one nano particle in film in all right doping stannic oxide, zinc paste, indium oxide, tantalum pentoxide, zirconium dioxide, 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.
In long-period gratings grid region, cladding surface prepares titanium dioxide nano-film, at titanium dioxide nano-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 the titanium dioxide nano-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 titanium dioxide nano-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 gratings surface film rapidly and accurately, regulate the thickness of nano thin-film rapidly and accurately, adjust long-period gratings rapidly and accurately to the sensitive range of different refractivity.
(3) the inventive method, compared with electrostatic layer by layer self-assembling method, the coating process of adjustment long-period gratings 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 gratings 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.
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 titanium dioxide nano-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 titanium dioxide nano-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
Prepare aqueous solution and the 0.2 mol/L boron aqueous acid of 0.1mol/L ammonium hexa-fluorotitanate respectively, subsequently by two kinds of solution equal-volume mixing, stirring makes mixed liquor mix, and with the ammoniacal liquor of 0.01mol/L, the pH of mixed solution is adjusted to 3.9, joined mixed liquor is poured into the reactive tank 2 of long-period gratings stationary installation 1, temperature of reaction is transferred to 50 DEG C, reaction is stopped when reaching 40min when reacted, and rinse 6 times with redistilled water, the now refractive index sensitivity of long period fiber grating 3 pairs of ethanol reaches 3300nm/RIU, improve 56 times than sensitivity when not growing titanium dioxide nano-film.
Embodiment 2
Titanium tetrachloride is joined in the hydrochloric acid of 1mol/L, be mixed with the titanium tetrachloride solution that concentration is 0.5mol/L, stir, joined solution 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, 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 normal butyl alcohols reaches 3500nm/RIU, improves 115 times than sensitivity when not growing titanium dioxide nano-film.
Embodiment 3
Prepare the aqueous solution of 0.001 mol/L titanium tetrafluoride, be 2.88 by the pH value of the watery hydrochloric acid adjustment solution of 0.01mol/L, stir.The solution prepared is poured into the reactive tank 2 of long-period gratings stationary installation 1, the temperature of solution is adjusted to 130 DEG C, constant temperature makes it reaction, reaction is stopped after 50 minutes, and repeatedly rinse with redistilled water, the now refractive index sensitivity of long period fiber grating 3 pairs of isopropyl alcohols reaches 1994nm/RIU, improves 39 times than sensitivity when not growing titanium dioxide nano-film.
Embodiment 4
Titanyl sulfate is joined in 0.1mol/L hydrochloric acid solution, be mixed with 100ml0.01mol/L titanyl sulfate solution, stir about 1 hour, then add the aqueous solution of 5 0.01mol/L urea, stir and make it abundant mixing.The solution prepared is poured into the reactive tank 2 of long-period gratings stationary installation 1, the temperature of solution is transferred to 80 DEG C, constant temperature is kept to make it reaction, when being reacted to 1.5h, stop reaction, and repeatedly rinse with redistilled water, the now refractive index sensitivity of long period fiber grating 3 pairs of water reaches 1500nm/RIU, improves 23 times than sensitivity when not growing titanium dioxide nano-film.
Claims (10)
1. a method for fast regulation and control long period fiber grating refractive index sensitivity, is characterized in that, by the method for liquid deposition at long-period gratings surface deposition titanium dioxide nano-film.
2. the method for a kind of quick regulation and control long period fiber grating refractive index according to claim 1 sensitivity, it is characterized in that: after stretching for long period fiber grating fixing, be added in the liquid of grating surface growth titanium dioxide nano-film, by controlling time and the temperature of the kind of reaction reagent in reaction solution, concentration and reaction solution, control the thickness of titanium dioxide nano-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.
3. the method for a kind of quick regulation and control long period fiber grating refractive index according to claim 1 sensitivity, is characterized in that: comprise the following steps:
The solution of (a) preparation growth titanium dioxide nano-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 titanium dioxide nano-film prepared and fixes in the reactive tank of long-period gratings;
E (), to the solution heating in reactive tank, controls temperature of reaction, titanium dioxide nano-film is increased on long-period gratings surface;
F () controls the time of reaction, control the growth thickness of titanium dioxide nano-film with this, and then adjustment long-period gratings is to the sensitive range of different refractivity, stops reaction when the sensitivity of long-period gratings refractive index reaches necessary requirement;
G () has the long-period gratings of titanium dioxide nano-film to rinse with redistilled water to growth, remove unreacted liquid and impurity.
4. the method for a kind of quick regulation and control long period fiber grating refractive index according to claim 3 sensitivity, is characterized in that: the solution of preparation growth titanium dioxide nano-film is at least one in titanium tetrafluoride, titanium tetrachloride, titanyl sulfate or the mixed solution for ammonium hexa-fluorotitanate and boric acid in step (a).
5. the method for a kind of quick regulation and control long period fiber grating refractive index according to claim 4 sensitivity, is characterized in that: the concentration of aqueous solution of titanium tetrafluoride, titanium tetrachloride, titanyl sulfate or ammonium hexa-fluorotitanate is 0.0001 ~ 10 mol/L.
6. the method for a kind of quick regulation and control long period fiber grating refractive index according to claim 5 sensitivity, is characterized in that: in step (a), and when reactant liquor is made up of ammonium hexa-fluorotitanate and boric acid, ammonium hexa-fluorotitanate, boric acid mol ratio are 1:0.5 ~ 50.
7. the method for a kind of quick regulation and control long period fiber grating refractive index according to claim 3 sensitivity, 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. the method for a kind of quick regulation and control long period fiber grating refractive index according to claim 3 sensitivity, is characterized in that: in step (e), range of reaction temperature is 20 ~ 180 DEG C.
9. the method for a kind of quick regulation and control long period fiber grating refractive index according to claim 1 sensitivity, it is characterized in that: in long-period gratings grid region, cladding surface prepares titanium dioxide nano-film, at least one nano particle in film in doping stannic oxide, zinc paste, indium oxide, tantalum pentoxide, zirconium dioxide, 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.
10. the method for a kind of quick regulation and control long period fiber grating refractive index according to claim 1 sensitivity, it is characterized in that: in long-period gratings grid region, cladding surface prepares titanium dioxide nano-film, at titanium dioxide nano-film surface fixed function identification material.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982427A (en) * | 2018-10-15 | 2018-12-11 | 中国计量大学 | Spherical welding long-period fiber grating surface plasma body resonant vibration hydrogen sensor |
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| US20070025661A1 (en) * | 2005-04-04 | 2007-02-01 | Zhiyong Wang | Fiber-optic sensor or modulator using tuning of long period gratings with self-assembled layers |
| CN101762564A (en) * | 2009-12-25 | 2010-06-30 | 北京理工大学 | Biochemical sensor based on thin-covering layer long-period fiber grating coupling resonant cavity |
| CN202433123U (en) * | 2012-02-11 | 2012-09-12 | 宁波工程学院 | Device using long period fiber Bragg grating to measure temperatures and refractive indexes in real time |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070025661A1 (en) * | 2005-04-04 | 2007-02-01 | Zhiyong Wang | Fiber-optic sensor or modulator using tuning of long period gratings with self-assembled layers |
| CN101762564A (en) * | 2009-12-25 | 2010-06-30 | 北京理工大学 | Biochemical sensor based on thin-covering layer long-period fiber grating coupling resonant cavity |
| CN202433123U (en) * | 2012-02-11 | 2012-09-12 | 宁波工程学院 | Device using long period fiber Bragg grating to measure temperatures and refractive indexes in real time |
Non-Patent Citations (4)
| Title |
|---|
| L. COELHO等: "《Enhanced refractive index sensing characteristics of optical fibre long period grating coated with titanium dioxide thin films》", 《SENSORS ANDACTUATORSB:CHEMICAL》 * |
| QIU-SHUN LI等: "《Improved detecting sensitivity of long period fiber gratings by polyelectrolyte multilayers:The effect of film structures》", 《OPTICSCOMMUNICATIONS》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108982427A (en) * | 2018-10-15 | 2018-12-11 | 中国计量大学 | Spherical welding long-period fiber grating surface plasma body resonant vibration hydrogen sensor |
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