CN102023029A - Miniature high-sensitivity optical fiber chemical sensor - Google Patents
Miniature high-sensitivity optical fiber chemical sensor Download PDFInfo
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Abstract
The invention relates to a miniature high-sensitivity optical fiber chemical sensor, belonging to the technical field of the miniature sensor. The chemical sensor particularly contains a fiber taper, an optical fiber resonant cavity, a top cover and a base, wherein the optical fiber resonant cavity is a single mode fiber without a coating layer and the middle part of the single mode fiber is plated with a zeolite membrane, thus the selective adsorption ability of the chemical sensor can be effectively increased. The chemical sensor adopts the fiber taper as stimulating waveguide to stimulate the whispering gallery chamber of the resonant cavity and has high coupling efficiency. The selective absorption effect of the zeolite coating is utilized to detect gas molecules with certain sizes. The base and top cover which are used as the loading device have simple structure and are prepared by the standard mechanical processing technology. The sensor in the invention can realize high sensitivity and high precision detection; the sensor can be used to detect the existence and concentration of a certain type of molecules in the environment; and the sensor can be widely applied in the fields such as environmental control, industrial process treatment, mine production, public safety devices and homeland security, and the sensitivity of the sensor can reach the ppm-order or even the ppb-order.
Description
Technical field
The present invention relates to a kind of micro high sensitivity fibre optic chemical sensor, belong to the microsensor technical field.
Background technology
Optical resonator structures commonly used has dish, ring, post, ball etc., and these solid of revolution resonator cavitys are supported the whispering gallery modes (whispering gallery modes is called for short WGMs) of high quality factor.WGMs is a kind of resonant optical mode that depends on pattern resonance, and the resonance frequency of this pattern (or wavelength) depends on the inside and outside index distribution of size and chamber of resonator cavity.Excite the waveguide common structure of resonator cavity WGM that (Ilchenko V S such as optical taper, prism, side polishing fibre are arranged by evanscent field, et al.Optical Resonators With Whispering-Gallery Modes--Part II:Applications.IEEE, Journal of Selected Topics in Quantum Electronics, 12 (1): 15-32,2006).Also the someone proposes to excite resonator cavity WGM with long period fiber grating (LPFG), but polishes the same too low defective of launching efficiency that exists of fine mode with prism, side.The coupling efficiency of optical taper (the several microns of diameter) is high, reaches as high as 99.9%.
Chemical sensor based on ball/dish/resonator cavitys such as ring/post, can realize detection (the Hanumegowda N M of extremely low concentration, et al.Refractometric sensors based on microsphere resonators, Applied Physics Letters, 87 (201107): 1-3,2005), still can not realize the selectivity of specific sized molecules is detected.By can realize the detection of specific sized molecules in resonator cavity surface plating one deck zeolite membrane, the zeolite membrane that plates is a kind of aluminosilicate of crystal type, have regular in the crystal structure and uniform duct, the aperture is the order of magnitude (being generally less than 1 nanometer) of molecular diameter, only allow the diameter molecule littler to enter, therefore the molecule in the potpourri can be sieved by size than the aperture.Utilize this characteristic, zeolite can be prepared into thickness is micron-sized film molecular sieve, and the detected material molecule is adsorbed selectively because of big or small and shape, causes the optical texture of zeolite pore and optical property to change (for example, refractive index changes).And the resonance frequency (or wavelength) of claustra pattern is very responsive to the change of zeolite membrane refractive index in the resonator cavity, thereby can realize supersensitive chemical sensor.
Summary of the invention
The objective of the invention is to use the detection problem of optical resonance cavity sensor, a kind of micro high sensitivity fibre optic chemical sensor that selectivity absorbs that has is provided specific big or small gas molecule for solving.
Micro high sensitivity fibre optic chemical sensor of the present invention comprises optical taper, fiber resonance cavity, top cover and base.
Described optical taper is the coat that single-mode fiber is removed center section, and the transition portion that forms awl waist, awl waist and two ends infrared optical fiber that is tapered in the middle part of optical fiber under the effect of high temperature heating and two ends pulling force presents taper; Its diameter requires to make the phase place of claustra mould in interior basic mode of optical taper and the resonator cavity to mate; According to manufacture craft and user demand, the most preferable diameter of thin part is the 1-2 micron.Optical taper has very high coupling efficiency, can excite the whispering gallery formula (WGMs) of resonator cavity.One end of optical taper is the light source input end; The other end is the transducing signal test side, is used to detect the situation of change of output light.
Described fiber resonance cavity is the single-mode fiber (removing coat) that the middle part is coated with zeolite membrane, can effectively strengthen the selective adsorption capacity of chemical sensor.The small pore of zeolite makes it have very big surface area/mass ratio, and this character makes its molecule of the detected material of absorption from surrounding environment effectively, and its gathering is concentrated in together.The molecule of detected material is adsorbed on the fiber resonance cavity surface according to its size selectively with the different of shape, in addition, being directed of molecule of the thing to be detected that is adsorbed in the zeolite pore and Methodistic arrangement, thus make the optical texture of zeolite pore and optical property change.
The cross-sectional sizes of described top cover is the same with base, has designed and produced sample storage chamber and mounting hole on it.
Optical taper groove, optical fibre resonator groove, sample storage chamber, flow channel, flow pass and mounting hole have been designed on the described base; It act as fixed fiber awl and fiber resonance cavity, guarantees that the two has good verticality, and provides an airtight testing environment for tested gas.Wherein, the sample storage chamber is the groove at base center; Optical taper groove and fiber resonance cavity groove are positioned at the base edge, and the shape size makes the groove inwall tangent with the circular surface of the infrared optical fiber of optical taper and fiber resonance cavity respectively; The number of the mounting hole on mounting hole and the top cover and position consistency are used for fixing top cover and base; Flow channel, flow pass lay respectively at the both sides in the base edge, are used for inflow, the outflow of tested gas.
The annexation of fibre optic chemical sensor each several part of the present invention is: the zeolite membrane at the awl waist of optical taper and fiber resonance cavity middle part contacts and is vertical; Optical taper is placed on the optical taper groove of base, and fiber resonance cavity is placed on the fiber resonance cavity groove of base; Top cover and base are fixed together by mounting hole with bolt.
The course of work of fibre optic chemical sensor of the present invention is: the light source input end of optical taper is connected external light source, and the transducing signal test side connects the light intensity checkout equipment.After the light of certain wave band incides optical fiber, after wherein the light of some wavelength has satisfied the phase matching of optical taper and fiber resonance cavity transmission mode, between optical taper and fiber resonance cavity resonance coupling takes place, and be transferred to the fiber resonance cavity from optical taper, the transmission loss of portion's scattering within it then.When sensor was in the environment of specific big or small gas molecule, the zeolite membrane on fiber resonance cavity surface can play the effect of adsorption gas molecule, and the coupled mode of optical taper and fiber resonance cavity also will change thereupon, thereby cause resonance wavelength to change.The light intensity checkout equipment is measured central resonance wavelength drift value, after experimental data is made finishing analysis and demarcated, obtains feeding back the parameter that extraneous factor changes, thereby reaches the sensing effect.
Beneficial effect
The present invention adopts optical taper as exciting waveguide to excite the whispering gallery formula (WGMs) of resonator cavity, has very high coupling efficiency.By the selective absorption of zeolite coating, can realize detection to the gas molecule of specific size.Base and cap structure as bogey are simple, only need the preparation of standard mechanical processing technology.Sensor of the present invention can be realized high sensitivity, high Precision Detection; The existence and the concentration (as explosive steam, tunnel gas molecule) that can be used for particular types molecule in the testing environment; Can be widely used in fields such as environment control, industrial process processing, mine production, public safety facility, Homeland Security, sensitivity can reach ppm even ppb magnitude.
Description of drawings
Fig. 1 is the structural representation of the fibre optic chemical sensor in the embodiment;
Fig. 2 is that the optical taper in the embodiment and the structure and the position of fiber resonance cavity concern synoptic diagram;
Fig. 3 is the understructure figure in the embodiment;
Fig. 4 is the cap structure figure in the embodiment;
Fig. 5 is a spectrum change synoptic diagram when detecting in the embodiment;
Fig. 6 is that resonance wavelength in the embodiment is with the theoretical modeling figure of refraction index changing;
Fig. 7 is that the zeolite refractive index in the embodiment changes lab diagram with the isopropyl alcohol gas concentration in nitrogen environment.
Label declaration
The 1-optical taper, 2-fiber resonance cavity, 3-top cover, the 4-base, 5-zeolite membrane, 6-optical taper input end, 7-optical taper output terminal, 8-flow channel, 9-flow pass, 10-optical taper groove, 11-fiber resonance cavity groove, 12-base sample storage chamber, 13-top cover sample storage chamber, 14-base mounting hole, 15-top cover mounting hole, 16-infrared optical fiber.
Embodiment
For objects and advantages of the present invention are described better, the invention will be further described below in conjunction with drawings and Examples.
The general structure of the fibre optic chemical sensor of present embodiment comprises optical taper 1, fiber resonance cavity 2, top cover 3 and base 4 as shown in Figure 1.
Wherein, optical taper 1 and fiber resonance cavity 2 select for use the single-mode fiber of Corning company to make, as shown in Figure 2.
The preparation of optical taper 1: single-mode fiber is placed on draws in the awl machine, start behind the setup parameter and draw the awl program, draw the optical fiber behind the awl to become the certain taper shape, the awl waist diameter 1-2um of place.
The preparation of the fiber resonance cavity 2 of plating zeolite membrane 5: get a single-mode fiber, remove the coat of center section with hoe scaler, TPAOH (the tetrapropyl ammonia oxyhydroxide) solution of 6.56ml, TEOS (ethyl orthosilicate) solution and the 30ml distilled water of 15.3ml are mixed, stirred 3 hours down at 50 ℃.Place mixed liquor to be placed into synthesis reactor then the optical fiber of handling, the length that places mixed liquor is the 12-15 millimeter.In baking oven, be preheating to 180 ℃, at 12 hours synthetic zeolite films of 180 ℃ of following hydro-thermals.After cleaning with distilled water, the fiber resonance cavity of plated film carried out 5 minutes ultrasonic bath.Afterwards above-mentioned coating process is come again to increase the thickness of zeolite membrane 5.At last will be the fiber resonance cavity 2 of plated film in baking oven, 80 ℃ of oven dry after 10 hours down, (temperature rate is 2 ℃/min) roasting 3 hours, has obtained the fiber resonance cavity 2 of zeolite molecular sieve plated film at last, and thickness is about 2.5 μ m in air under 500 ℃.
Top cover 3 (as shown in Figure 4) and base 4 (as shown in Figure 3) adopt the organic glass of 3cm * 3cm * 1cm to process.Get out the through hole of placing bolt at four drift angle places, process the sample storage chamber (13 and 12) of the tested gas of 1cm * 1cm * 0.5cm respectively at top cover 3 and base 4 middle parts, and dig out flow channel 8 and flow pass 9 in base 4 both sides, process the U type groove (optical taper groove 10 and fiber resonance cavity groove 11) of placing optical taper 1 and fiber resonance cavity 2 with the ultraprecise milling cutter at base 4 at last, cross sectional dimensions is 150um * 150um.
When the sensor of this case making is used for the specific gas Molecular Detection, when wavelength continually varying incident light enters into the coupled zone of fiber resonance cavity 2 and optical taper awl waist from the incident end 6 of optical taper 1, the light of some specific wavelength forms whispering gallery modes in the fiber resonance cavity 2 that is coated with zeolite membrane 5, " transmissivity-wavelength " curve of output terminal 7 output spectrums will produce a series of resonance absorption bands (as shown in Figure 5), and the wavelength of these resonant belt correspondences is very responsive to the variations in refractive index of zeolite coatings.Detected gas molecule in fiber resonance cavity 2 absorption environment, the refractive index of zeolite membrane 5 changes, and variation has also taken place in the resonance wavelength of whispering gallery modes in the fiber resonance cavity 2.According to the size that resonance wavelength moves, can obtain the change amount (as shown in Figure 6) of refractive index.Fig. 6 is the Theoretical Calculation result: scribble near the fiber resonance cavity 2 interior claustra moulds of wavelength 1550nm of different-thickness (h) zeolite coating, its resonance wavelength moves the relation between (δ λ) and the zeolite coating refraction index changing amount (δ n).Slope of a curve is promptly represented the sensitivity S=δ λ/δ n of sensor, and unit is nm/RIU (RIU:Refractive Index Unit, an expression refractive index unit).Can be drawn by Fig. 6, the zeolite coating can greatly improve the sensitivity of sensor, for example: when not having the zeolite coating (h=0 μ m), transducer sensitivity S ≈ 26.7nm/RIU; When the zeolite coating thickness surpasses 3 microns (h 〉=3 μ m), transducer sensitivity S ≈ 1136.3nm/RIU has improved about 43 times, far above the traditional optical resonator sensor.Simultaneously, when the zeolite coating thickness surpasses 3 microns, sensor has good linear characteristic, and is very convenient in actual applications.In actual measurement, the change of refractive index is answered material molecule concentration corresponding (as shown in Figure 7) with environmental facies, can detect the concentration of the chemical molecular of surveying in the specific gas thus.Fig. 7 be zeolite refractive index (n) in nitrogen environment with isopropyl alcohol gas molecule concentration (C
Ip) change curve.When isopropyl alcohol gas molecule concentration reaches 1000ppm, the zeolite refractive index is increased to 1.396 by 1.336, be δ n=0.06RIU, for scribbling the fiber resonance cavity that thickness surpasses 3 micron zeolite layers, the resonance wavelength of its Whispering-gallery-mode is with mobile δ λ=S * δ n=1136.3 * 0.0668nm.And tunable laser resolution is far smaller than 1nm at present, and therefore, this sensor can be realized the detection to the ppm magnitude of isopropyl alcohol gas molecule fully, even can reach the ppb magnitude.
Above-described specific descriptions; purpose, technical scheme and beneficial effect to invention further describe, and institute it should be understood that the above only is specific embodiments of the invention; be used to explain the present invention, and be not intended to limit the scope of the invention.Those skilled in the art also can do other variations in spirit of the present invention.But, within the spirit and principles in the present invention all, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. a micro high sensitivity fibre optic chemical sensor is characterized in that: comprise optical taper, fiber resonance cavity, top cover and base;
Described optical taper is the coat that single-mode fiber is removed center section, and the transition portion that forms awl waist, awl waist and two ends infrared optical fiber that is tapered in the middle part of optical fiber under the effect of high temperature heating and two ends pulling force presents taper; Its diameter requires to make the phase place of claustra mould in interior basic mode of optical taper and the resonator cavity to mate; Optical taper has very high coupling efficiency, can excite the whispering gallery formula of resonator cavity; One end of optical taper is the light source input end; The other end is the transducing signal test side, is used to detect the situation of change of output light;
Described fiber resonance cavity is that the middle part is coated with zeolite membrane and removes the single-mode fiber of coat, can effectively strengthen the selective adsorption capacity of chemical sensor; The small pore of zeolite makes it have very big surface area/mass ratio, can adsorb the molecule of detected material effectively from surrounding environment, and its gathering is concentrated in together; The molecule of detected material is adsorbed on the fiber resonance cavity surface according to size selectively with the different of shape, and being directed and Methodistic arrangement, makes the optical texture of zeolite pore and optical property change;
The cross-sectional sizes of described top cover is the same with base, has designed and produced sample storage chamber and mounting hole on it;
Optical taper groove, optical fibre resonator groove, sample storage chamber, flow channel, flow pass and mounting hole have been designed on the described base; Be used for fixing optical taper and fiber resonance cavity, and provide an airtight testing environment for tested gas;
The annexation of each part mentioned above is: the zeolite membrane at the awl waist of optical taper and fiber resonance cavity middle part contacts and is vertical; Optical taper is placed on the optical taper groove of base, and fiber resonance cavity is placed on the fiber resonance cavity groove of base; Top cover and base are fixed together by mounting hole with bolt.
2. a kind of micro high sensitivity fibre optic chemical sensor according to claim 1 is characterized in that: the described optical taper the most preferred diameter of thin part is the 1-2 micron.
3. a kind of micro high sensitivity fibre optic chemical sensor according to claim 1 is characterized in that: the sample storage chamber of described base is the groove at base center; Optical taper groove and fiber resonance cavity groove are positioned at the base edge, and the shape size makes the groove inwall tangent with the circular surface of the infrared optical fiber of optical taper and fiber resonance cavity respectively; The number of the mounting hole on mounting hole and the top cover and position consistency are used for fixing top cover and base; Flow channel, flow pass lay respectively at the both sides in the base edge, are used for inflow, the outflow of tested gas.
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Cited By (10)
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| CN106635773A (en) * | 2016-09-29 | 2017-05-10 | 南开大学 | DNA (Deoxyribonucleic Acid) hybridized micro-fluidic detector based on optical fiber micro-cavity echo wall |
| CN107121157A (en) * | 2017-05-04 | 2017-09-01 | 重庆大学 | Couple the measurement filter of optical fiber and Echo Wall microcavity |
| CN107941716A (en) * | 2017-12-29 | 2018-04-20 | 首都师范大学 | Multi-core optical fiber resonator gas sensor |
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| CN109708675A (en) * | 2018-12-13 | 2019-05-03 | 云南电网有限责任公司电力科学研究院 | A kind of fibre optical sensor based on helmholtz resonance device |
| CN110262155A (en) * | 2019-08-13 | 2019-09-20 | 南京南智先进光电集成技术研究院有限公司 | A kind of echo wall-shaped chamber position matches system and method |
| CN112504973A (en) * | 2020-10-14 | 2021-03-16 | 杭州香侬科技有限公司 | Self-referencing optical micro-resonator sensor |
| CN112577426A (en) * | 2020-11-30 | 2021-03-30 | 中国科学院长春光学精密机械与物理研究所 | Axial probe type sensing test method |
| CN112945904A (en) * | 2021-01-22 | 2021-06-11 | 中新苏州工业园区清城环境发展有限公司 | Hydrocarbon optical fiber chemical detection probe and preparation method thereof |
| CN114966985A (en) * | 2022-06-01 | 2022-08-30 | 暨南大学 | Optical fiber humidity sensor and manufacturing method thereof |
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| CN106635773A (en) * | 2016-09-29 | 2017-05-10 | 南开大学 | DNA (Deoxyribonucleic Acid) hybridized micro-fluidic detector based on optical fiber micro-cavity echo wall |
| CN107121157A (en) * | 2017-05-04 | 2017-09-01 | 重庆大学 | Couple the measurement filter of optical fiber and Echo Wall microcavity |
| CN107941716A (en) * | 2017-12-29 | 2018-04-20 | 首都师范大学 | Multi-core optical fiber resonator gas sensor |
| CN107941716B (en) * | 2017-12-29 | 2024-01-02 | 首都师范大学 | Multi-core optical fiber resonant cavity gas sensor |
| CN109142271A (en) * | 2018-07-16 | 2019-01-04 | 哈尔滨工程大学 | A kind of light fibre humidity transducer and preparation method thereof of combination spider egg-case silk |
| CN109142271B (en) * | 2018-07-16 | 2020-12-04 | 哈尔滨工程大学 | Optical fiber humidity sensor combined with spider egg-wrapped silk and manufacturing method thereof |
| CN109708675B (en) * | 2018-12-13 | 2021-02-26 | 云南电网有限责任公司电力科学研究院 | Optical fiber sensor based on Helmholtz resonator |
| CN109708675A (en) * | 2018-12-13 | 2019-05-03 | 云南电网有限责任公司电力科学研究院 | A kind of fibre optical sensor based on helmholtz resonance device |
| WO2021027062A1 (en) * | 2019-08-13 | 2021-02-18 | 南京南智先进光电集成技术研究院有限公司 | Echo wall cavity phase matching system and method |
| GB2587313A (en) * | 2019-08-13 | 2021-03-24 | Nanjing Nanzhi Advanced Photoelectric Integrated Tech Research Institute Co Ltd | Phase matching system and method for whispering-gallery-mode cavity |
| GB2587313B (en) * | 2019-08-13 | 2021-12-01 | Nanjing Nanzhi Advanced Photoelectric Integrated Tech Research Institute Co Ltd | Phase matching system and method for whispering-gallery-mode cavity |
| CN110262155A (en) * | 2019-08-13 | 2019-09-20 | 南京南智先进光电集成技术研究院有限公司 | A kind of echo wall-shaped chamber position matches system and method |
| CN112504973A (en) * | 2020-10-14 | 2021-03-16 | 杭州香侬科技有限公司 | Self-referencing optical micro-resonator sensor |
| CN112577426A (en) * | 2020-11-30 | 2021-03-30 | 中国科学院长春光学精密机械与物理研究所 | Axial probe type sensing test method |
| CN112945904A (en) * | 2021-01-22 | 2021-06-11 | 中新苏州工业园区清城环境发展有限公司 | Hydrocarbon optical fiber chemical detection probe and preparation method thereof |
| CN114966985A (en) * | 2022-06-01 | 2022-08-30 | 暨南大学 | Optical fiber humidity sensor and manufacturing method thereof |
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Application publication date: 20110420 |