CN109163759A - The reflective nitrate concentration of all -fiber and temperature simultaneously measuring device - Google Patents
The reflective nitrate concentration of all -fiber and temperature simultaneously measuring device Download PDFInfo
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- CN109163759A CN109163759A CN201811029317.2A CN201811029317A CN109163759A CN 109163759 A CN109163759 A CN 109163759A CN 201811029317 A CN201811029317 A CN 201811029317A CN 109163759 A CN109163759 A CN 109163759A
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Abstract
The invention belongs to technical field of optical fiber sensing, disclose a kind of reflective nitrate concentration of all -fiber and temperature simultaneously measuring device, including host computer, spectrometer, y-type optical fiber, sensing unit and light source, sensing unit is cascaded by multimode fibre and single mode optical fiber, wherein, multimode fibre one end connects with y-type optical fiber, the multimode fibre other end and the coaxial welding of single mode optical fiber, it is coated with to single mode optical fiber outer surface and end face all standing golden film, nitrate anion sensitive membrane is coated with outside the golden film of outer surface；Outside nitrate anion sensitive membrane, begins axially to stop to single mode optical fiber half extension position along single mode optical fiber from welding end, be coated with temperature-sensitive membrane.Not only preparation process is simple by the present invention, at low cost, stable structure, but also passes through while measuring nitrate concentration and temperature, can effectively reduce influence of the temperature to nitrate concentration measurement accuracy.
Description
Technical field
The invention belongs to technical field of optical fiber sensing, it is related to a kind of reflective nitrate concentration of all -fiber and temperature while surveys
Measure device.
Background technique
Water pollution problems, which has become countries in the world all, needs one of problem faced, and the nitrate in water body is a kind of main
Pollutant, excessive nitrate is mainly from industrial wastewater in usual water, and rotting etc. for pollution by chemical fertilizer and swill is excessive
Nitrate can to biology existence impact [Sevda S, Sreekishnan T R, Pous N, et
al.Bioelectroremediation of perchlorate and nitrate contaminated water:A
review[J].Bioresource technology,2018.].Currently, the main method of detection nitrate concentration has cadmium column also
Former method, ionic association constant and the chromatography of ions, but these method equipment are expensive, it is cumbersome, and be easy to be interfered.Optical fiber
The advantages that sensing technology has high sensitivity, and response is rapid, can be with on-line measurement, it is most important that it can be dry to avoid electromagnetism
It disturbs, becomes important branch [Wei Y, Liu C, Zhang Y, the et al.Multi-channel SPR of sensory field
sensor based on the cascade application of the Single-mode and multimode
optical fiber[J].Optics Communications,2017,390:82-87.]。
The method that fiber sensor measuring chemical concentration can be combined using fibre optical sensor with sensitive membrane.When to
The chemical component of survey reacts with sensitive membrane, will lead to refractive index at sensitive membrane and changes, utilizes fibre optical sensor doubling
The high sensitivity of rate is penetrated to realize the measurement of chemical concentration.The method master of refractive index is measured currently with fibre optical sensor
There are interference-type and SPR type sensor.Interferometric sensor is broadly divided into Fabry Perot interference sensor, Mach-Zehnder
Interference sensor and Michelson interference sensor, this kind of sensors are the interference phenomenon according to light and the optical fiber being derived
The interference spectrum of sensor, light can change with the variation of refractive index, to realize refractometry [Yang J, Yang
M,Guan C Y,et al.In-fiber Mach-Zehnder interferometer with piecewise
interference spectrum based on hole-assisted dual-core fiber for refractive
Index sensing [J] .Optics express, 2018,26 (15): 19091-19099.], but interference-type optical fiber senses
The sensitivity of device impact of refractive index measurement is relatively low.And this kind of sensor can be often subject to other extraneous items when carrying out actual measurement
The interference of part, interference spectrum can not only change with the change of refractive index, and temperature also results in interference spectrum and moves
It is dynamic, it can impact of refractive index measurement generation interference.SPR type sensor be numerous scholars research in recent years hot spot [Yinquan,
Y.Investigation for terminal reflection optical fiber SPR glucose sensor and
glucose sensitive membrane with immobilized GODs[J].Optics Express,2017,25
(4):3884-3898.].The resonance wavelength of such sensor can be moved with the change of refractive index, and then realize refraction
The measurement of rate.And its refractometry high sensitivity is in interferometric sensor.However, the measuring signal of this kind of sensor is same
It will receive the interference of temperature.
To sum up, the refractometry sensor based on optical fiber at present there are still by temperature interference the problem of.It is the most key
, the sensor of performance current to(for) nitrate concentration and temperature simultaneously measuring is still without reaching ideal degree.
Summary of the invention
It is an object of the invention to overcome the nitrate concentration measurement sensor currently based on optical fiber to be affected by temperature not
Foot place, proposes a kind of reflective nitrate concentration of simple, at low cost, stable structure all -fiber of preparation process and temperature simultaneously
Measuring device.
The specific technical proposal is:
The reflective nitrate concentration of all -fiber and temperature simultaneously measuring device, including host computer, spectrometer, y-type optical fiber, biography
Sense unit and light source, sensing unit are connect with light source and spectrometer respectively through y-type optical fiber, and spectrometer is connect with host computer；It is described
Sensing unit is cascaded by multimode fibre and single mode optical fiber, wherein multimode fibre one end connects with y-type optical fiber, multimode fibre
Golden film is coated with to the other end and the coaxial welding of single mode optical fiber, single mode optical fiber outer surface and end face all standing, outside the golden film of outer surface
It is coated with nitrate anion sensitive membrane；Outside nitrate anion sensitive membrane, begin from welding end axial to single mode optical fiber half length along single mode optical fiber
Position is stopped, and temperature-sensitive membrane is coated with.
The light that light source issues enters in single mode optical fiber after y-type optical fiber is transmitted to multimode fibre, and table is inspired in golden film
Surface plasma resonance.Nitrate anion sensitive membrane is coated with outside golden film, and the outer half length of nitrate anion sensitive membrane is by temperature-sensitive membrane
Covering, output spectrum will generate the different resonance paddy of two resonance wavelengths, finally, reflected by single mode optical fiber end face
Optical signal enters spectrometer via y-type optical fiber, and sends data to host computer to observe the variation of output map；Work as nitrate anion
When concentration changes, the refractive index of the outer nitrate anion sensitive membrane of golden film can be changed, make the resonance wave of the corresponding resonance paddy of nitrate concentration
Length moves, and when ambient temperature changes, can not only change the refractive index of temperature-sensitive membrane and then keep temperature corresponding
The resonance wavelength of resonance paddy moves, and the resonance wavelength of the corresponding resonance paddy of nitrate concentration can also moved, therefore,
Using the method for dual wavelength matrix, the amount of movement by observing two resonance paddy resonance wavelength counter can release nitrate concentration and
Temperature.
Further, above-mentioned single-mode optical fiber length is 10mm, and for golden film with a thickness of 40nm, temperature-sensitive membrane is poly dimethyl silicon
Siloxane film.
Further, above-mentioned nitrate anion sensitive membrane is made using carbon nano tube/copper nanoparticle composite membrane.
Further, the preparation flow of above-mentioned nitrate anion sensitive membrane are as follows: polyetherimide is added to 40~50mL first
It is made into 1wt% polyetherimide solution in methanol, then, 15~20mg multi-walled carbon nanotube is added and stirs, by the mixed liquor
Stratification after ultrasonic treatment 2~3 hours, then takes lower sediment to be dissolved in after 40~50mL methanol and carries out ultrasonic treatment 1~2 again
Hour simultaneously stirs evenly, and the copper chloride solution of the freshly prepd 0.1mol/L of 10~12mL next is added and 10~12mL concentration is
0.1mol/L sodium borohydride solution stir process adds the progress of 3~4mL chitosan solution after being finally centrifuged mixed liquor
Ultrasound and stir process obtain the solution for being used to prepare carbon nano tube/copper nanoparticle composite membrane, recycle dip-coating method will
It is plated in sensor surface, and each dip time is 20min, and is lifted three times, carries out under conditions of 90 DEG C after lifting every time
Annealing, the time made annealing treatment every time is 30min, so that carbon nano tube/copper nanoparticle composite membrane is coated in securely
Golden film outer surface.
It can be seen from the above technical proposal that the invention has the following advantages:
1) the reflective nitrate concentration of this all -fiber proposed by the present invention and temperature simultaneously measuring device, inherit tradition
Essential safety, electromagnetism interference possessed by fibre optical sensor, high temperature high voltage resistant, it is corrosion-resistant the advantages that；
2) the reflective nitrate concentration of this all -fiber proposed by the present invention and temperature simultaneously measuring device, not only prepare work
Skill is simple, at low cost, stable structure, and passes through while measuring nitrate concentration and temperature, can effectively reduce temperature to nitric acid
The influence of root measurement of concetration precision.
Detailed description of the invention
Fig. 1 is optical fibre sensor structure schematic diagram provided by the invention.
Fig. 2 is the relational graph of sensor difference dip time and resonance wavelength amount of movement.
The relational graph of Fig. 3 sensor difference lifting number and resonance wavelength amount of movement.
Fig. 4 sensor nitrate concentration measure spectrum curve.
Fig. 5 is sensor temperature measure spectrum curve.
Fig. 6 is that sensor nitrate concentration measures linearly interval matched curve.
Fig. 7 is sensor temperature measurement sensitivity curve.
In figure: 1 host computer；2 spectrometers；21 multimode fibres；22 PDMS membranes；23 carbon nano tube/copper nanometers
Particle composite membrane；24 golden films；25 single mode optical fibers；3Y type optical fiber；4 sensing units；5 light sources.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Attached drawing is described in further detail specific structure of the invention, principle and the course of work.
It is as shown in Figure 1 a kind of reflective nitrate concentration of all -fiber proposed by the present invention and temperature simultaneously measuring device.
Its course of work are as follows: the light that light source 5 issues enters single mode optical fiber 25 first after y-type optical fiber 3 is transmitted to multimode fibre 21, then
It reflects in 25 endface of single mode optical fiber into y-type optical fiber 3 and is transmitted to the monitoring that spectrometer 2 carries out spectroscopic studying amount.Wherein,
Welding is carried out by heat sealing machine between multimode fibre 21, single mode optical fiber 25, the length of single mode optical fiber 25 is 10mm, and single-mode optics
40nm golden film 24 is coated with outside fine, carbon nano tube/copper nanoparticle composite membrane 23, carbon nano tube/copper nanometer are plated in 24 outer surface of golden film
The half length areas of 23 external distance multimode fibre 21 of particle composite membrane is coated with PDMS membrane 22, dimethyl silicone polymer
The preparation of film 22 is mixed using three kinds of dimethyl silicone polymer, ethyl orthosilicate and dibutyl tin dilaurate reagents.Its
The mass ratio of middle dimethyl silicone polymer, ethyl orthosilicate and dibutyl tin dilaurate is 10:1:0.7.
When light is transferred to single mode optical fiber 25 from multimode fibre 21, due to the core diameter and single mode optical fiber of multimode fibre 21
25 core diameter gap is larger, and part light can be coupled into covering and be transmitted, a part at this moment transmitted in covering
Light can leak into the golden film 24 outside covering, and surface plasma body resonant vibration occurs, and lead to output spectrum generation energy loss defeated
Spectrum generates resonance paddy in certain wave strong point out, when extraneous nitrate concentration occurs mobile, the resonance wavelength of this resonance paddy
It can move, and then realize the measurement of nitrate concentration, when the outer half length quilt of carbon nano tube/copper nanoparticle composite membrane 23
After PDMS membrane 22 covers, medium a part outside carbon nano tube/copper nanoparticle composite membrane 23 just becomes
PDMS membrane 24, output spectrum will generate two resonance paddy at this time, respectively correspond nitrate concentration and temperature
Variation.The refractive index of PDMS membrane 22 can change with the variation of temperature, which achieves nitrate concentration and
Temperature simultaneously measuring.
In the present invention, carbon nano tube/copper nanoparticle composite membrane 23 is plated in sensor using dip-coating method technique
The final performance of sensor is influenced, the affecting parameters of dip-coating method plated film are mainly dip time and lifting number, when dipping
Between it is longer, the sensitive material for being attached to sensitive zones is also more；On the one hand lifting can often guarantee to increase sensitizing range
Sensitive material, on the other hand can guarantee the sensitive membrane for having more uniform.Firstly, single lifting processing is carried out to sensor,
Dip time is 5-30 minutes, and as shown in Figure 2 as a result, dip time is in 20min, sensor has maximum drift amount, therefore most
Choosing dip time eventually is 20min.Then repeatedly lifting operation being carried out to sensor, each dip time is all 20min, and
Sensor is annealed 30min under conditions of 90 DEG C after lifting every time.As shown in figure 3, with the increase of lifting number, sensor
More sensitive to the variation of nitrate concentration, sensitivity is higher, and when lifting number is three times, sensor wavelength amount of movement reaches
37nm.
In the present invention, PDMS membrane 24 is plated in 23 half length of carbon nano tube/copper nanoparticle composite membrane
Outside, when ambient temperature remains unchanged and nitrate anion changes, will lead to attachment on the carbon nanotubes by reducing nitrate radical
The ammonia concentration that reaction generates changes, and so that refractive index is changed, so that the resonance of the corresponding resonance paddy of nitrate concentration
Wavelength XnIt moves, as shown in Figure 4.And when nitrate concentration remains unchanged and temperature changes, can not only it change poly-
The refractive index of dimethyl siloxane film 22 and then the resonance wavelength for making the corresponding resonance paddy of temperatureTIt moves, can also make nitric acid
The resonance wavelength of the corresponding resonance paddy of root concentrationnIt moves, as shown in Figure 5.In conjunction with dual wavelength matrix method, can obtain:
Wherein, Δ λn、ΔλTRespectively salinity corresponds to the amount of movement of resonance paddy resonance wavelength and temperature corresponds to resonance paddy resonance
The amount of movement of wavelength amount of movement；Δ n, Δ T are respectively the variable quantity of nitrate concentration and the variable quantity of temperature.A is that nitrate anion is dense
Nitrate concentration corresponds to the motion sensitivity coefficient of resonance paddy resonance wavelength when degree variation；B, when d is respectively ambient temperature variation
Nitrate concentration corresponds to the motion sensitivity coefficient of resonance paddy resonance wavelength and temperature corresponds to the mobile spirit of resonance paddy resonance wavelength
Sensitivity coefficient.In the present invention, when the structural parameters of sensor probe are fixed, a, b, d are fixed value, the nitrate anion of sensor
Measurement of concetration sensitivity and temperature measurement sensitivity curve difference are as shown in Figure 6 and Figure 7, at this time the dual wavelength matrix of sensor
Are as follows:
Therefore wherein Δ m=Δ lgn can be obtained by formula (2), correspond to resonance paddy resonance wavelength by observing nitrate concentration
Amount of movement and temperature correspond to resonance paddy resonance wavelength amount of movement and counter can release nitrate concentration and temperature level, can not only solve
The certainly cross sensitivity problem that temperature measures nitrate concentration can also realize nitrate concentration and temperature while monitor, and be nitre
The high-acruracy survey of acid group concentration provides possibility.
Claims (6)
1. the reflective nitrate concentration of all -fiber and temperature simultaneously measuring device, including host computer, spectrometer, y-type optical fiber, sensing
Unit and light source, which is characterized in that sensing unit is connect with light source and spectrometer respectively through y-type optical fiber, spectrometer and host computer
Connection；The sensing unit is cascaded by multimode fibre and single mode optical fiber, wherein and multimode fibre one end connects with y-type optical fiber,
It is coated with golden film, outer surface to the multimode fibre other end and the coaxial welding of single mode optical fiber, single mode optical fiber outer surface and end face all standing
Golden film outside be coated with nitrate anion sensitive membrane；Outside nitrate anion sensitive membrane, begin from welding end axial to single mode optical fiber along single mode optical fiber
Half extension position is stopped, and temperature-sensitive membrane is coated with.
2. the reflective nitrate concentration of all -fiber according to claim 1 and temperature simultaneously measuring device, which is characterized in that
The nitrate anion sensitive membrane is made using carbon nano tube/copper nanoparticle composite membrane.
3. the reflective nitrate concentration of all -fiber according to claim 1 or 2 and temperature simultaneously measuring device, feature exist
In the preparation flow of the nitrate anion sensitive membrane are as follows: the polyetherimide of 1wt% and 15mg multi-walled carbon nanotube are added first
Stirred into 40mL~50mL methanol, stratification after mixed liquor is ultrasonically treated, then take lower sediment be dissolved in 40mL~
It is ultrasonically treated and is stirred evenly again after 50mL methanol, the copper chloride solution and 10mL of the 0.1mol/L of 10mL is next added
Concentration is 0.1mol/L sodium borohydride solution stir process, and 3mL~5mL chitosan is added after being finally centrifuged mixed liquor
Solution carries out ultrasound and stir process obtains the solution for being used to prepare carbon nano tube/copper nanoparticle composite membrane, recycles dipping
Czochralski method is plated in sensor surface, and each dip time is 20min, and is lifted three times, every time in 90 DEG C of item after lifting
It is made annealing treatment under part, the time made annealing treatment every time is 30min, so that carbon nano tube/copper nanoparticle composite membrane is secured
Ground is coated in golden film outer surface.
4. the reflective nitrate concentration of all -fiber according to claim 1 or 2 and temperature simultaneously measuring device, feature exist
In single-mode optical fiber length 10mm.
5. the reflective nitrate concentration of all -fiber according to claim 1 or 2 and temperature simultaneously measuring device, feature exist
In golden film is with a thickness of 40nm.
6. the reflective nitrate concentration of all -fiber according to claim 1 or 2 and temperature simultaneously measuring device, feature exist
In temperature-sensitive membrane is PDMS membrane.
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| CN112147082A (en) * | 2020-09-24 | 2020-12-29 | 杭州春来科技有限公司 | Vehicle-mounted urea monitoring device and monitoring method |
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