CN208568590U - A kind of refractive index detection system of index sensor and its composition - Google Patents
A kind of refractive index detection system of index sensor and its composition Download PDFInfo
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- CN208568590U CN208568590U CN201821236235.0U CN201821236235U CN208568590U CN 208568590 U CN208568590 U CN 208568590U CN 201821236235 U CN201821236235 U CN 201821236235U CN 208568590 U CN208568590 U CN 208568590U
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Abstract
The utility model relates to a kind of index sensor and its refractive index detection systems of composition.The index sensor includes a photonic crystal fiber and two single mode optical fibers, and the both ends of the photonic crystal fiber with a Single-Mode Fiber Coupling, and are respectively formed at two Coupling points a waist and expand optical fiber and slightly bore respectively;The photonic crystal fiber surface is coated with graphene layer.The index sensor of the utility model is based on graphene coated optical fiber and there is waist to expand double thick wimble structures of optical fiber as interferometer, is combined by optical fiber with graphene, changes the refractive index of optical fiber, improves its sensitivity;Coupling and compound, realization multiple-mode interfence using the thick wimble structures progress fibre core of the double optical fiber of waist expansion and cladding mode.The detection of liquids and gases material concentration is responded the index sensor of the utility model with High Linear and excellent sensitivity, and has the characteristics that at low cost, production method is simple, repeatability is high, can mass production use.
Description
Technical field
The utility model relates to sensor technical field more particularly to the refractive index of a kind of index sensor and its composition
Detection system.
Background technique
Graphene is the carbon homoatomic that hexagoinal lattice is arranged in by single layer of carbon atom as a kind of novel two-dimension nano materials
Obform body has the characteristics that high intensity, nearly transparent, large specific surface area, stability are high, can be used as adsorbent material.Photon is brilliant
There are a large amount of micro-structures inside body cross section of optic fibre so that can operating space it is big so that it is passed in optic communication, optical device and light
Extremely wide application is obtained in the various fields such as sense, it is the most prominent in sensory field of optic fibre application, there is electromagnetism interference
Ability is strong, insulating properties is high, can burn-proof and explosion prevention, flexibly flexible flexure, suitable for the New Sensing Technology of remote monitoring etc., it is especially suitable
Monitoring under the conditions of preferably severe and hazardous environment.Mach-Zender interferometer (Mach-Zehnder interferometer,
MZI) can be widely applied to measurement strain, temperature and refractive index, the principle of the device is the core mode and cladding mode of optical fiber
Between interference.The sensing substance of existing fibre optical sensor is simple optical fiber, sensitive when for material concentration detection
It spends to be improved.So far, graphene coating optical fiber and with waist amplification bipyramid core as Mach-Zehnder
The research work of interference index sensor is not yet reported that this index sensor can be applied to Concentration Testing.
Utility model content
Based on this, the purpose of the utility model is to provide a kind of index sensors, utilize the light of graphene coated
Fibre is used as sensing arrangement, is effectively applied to Concentration Testing.
The purpose of this utility model is achieved through the following technical solutions: a kind of index sensor, including a photon
Crystal optical fibre and two single mode optical fibers, the both ends of the photonic crystal fiber respectively with a Single-Mode Fiber Coupling, and in two couplings
Waist expansion optical fiber is respectively formed at chalaza slightly to bore;The photonic crystal fiber surface is coated with graphene layer.
Compared with the existing technology, the index sensor of the utility model is based on graphene coated optical fiber and has waist
Expand double thick wimble structures of optical fiber as interferometer, is combined by optical fiber with graphene, using the special construction of graphene to molten
Molecule in liquid has adsorptivity, thus changes the refractive index of optical fiber, improves its sensitivity;Expand double optical fiber using waist slightly to bore
The coupling of structure progress fibre core and cladding mode and compound, realization multiple-mode interfence.The index sensor of the utility model is for liquid
Body and gas species concentration detection have High Linear response and excellent sensitivity, and at low cost, production method is simple, can
The high feature of repeatability, can mass production use.
Further, the distance between described two Coupling point is 3.9~4.1cm.
Further, the waist expands a length of 395~405 μm of waist that optical fiber is slightly bored, and waist diameter is 179~180 μm.
Further, the distance between described two Coupling point is 4cm;The waist expands a length of 400 μ of waist that optical fiber is slightly bored
M, waist diameter are 179.25 μm.
Further, the graphene layer is 1~10 layer of graphene.
Further, the graphene layer is single-layer graphene, with a thickness of 0.33~0.35nm.
The present invention also provides a kind of refractive index detection systems, including index sensor of the present invention, light source, sample
Product room and signal processing system, the index sensor be set to the sample room in, both ends respectively with the light source and institute
State signal processing system connection.
Further, the signal processing system is spectroanalysis instrument.
In order to better understand and implement, according to the present invention will be described in detail below with reference to the accompanying drawings.
Detailed description of the invention
Fig. 1 is the schematic diagram of the index sensor of embodiment 1.
Fig. 2 is the compound film preparation and schematic diagram of transfer process of embodiment 1.
Fig. 3 is the surface topography map of the graphene coated optical fiber of embodiment 1.
Fig. 4 is the Raman spectrogram of the graphene coated optical fiber of embodiment 1.
Fig. 5 is the schematic diagram of the refractive index detection system of embodiment 1.
Fig. 6 is the spectrogram of various concentration sucrose solution and the linear relationship chart of sucrose concentration and trough.
Fig. 7 is the variation relation figure between the wavelength shift of formant and the refractive index of sucrose solution.
Fig. 8 is the spectrogram of various concentration hydrogen sulfide gas.
Fig. 9 is the linear relationship chart of concentration of hydrogen sulfide and trough.
Specific embodiment
The utility model proposes one kind based on graphene coated optical fiber and there are the double thick wimble structures of optical fiber of waist expansion to make
For the index sensor of interferometer, the novel refractometer based on all -fiber modal interference is illustrated, by being clipped in two single modes
Two waists formed by photonic crystal fiber (PCF) between optical fiber (SMF) expand fusion occluder and constitute, in addition, graphite
Sensing membrane of the alkene as the covering outer surface PCF.The sensor of the utility model is effectively applied to such as sucrose solution, vulcanization
The Concentration Testing of hydrogen.
Embodiment 1
Referring to Fig. 1, its schematic diagram for the index sensor of the present embodiment.The index sensor 10 includes one
Photonic crystal fiber 11 and two single mode optical fibers 12, the both ends of the photonic crystal fiber 11 respectively with 12 coupling of single mode optical fiber
It closes, and is respectively formed waist expansion optical fiber at two Coupling points and slightly bores 13;12 surface of photonic crystal fiber is coated with stone
Black alkene layer.Preferably, the distance between described two Coupling point is 3.9~4.1cm;It is a length of that the waist expands the waist that optical fiber is slightly bored
395~405 μm, waist diameter is 179~180 μm;The graphene layer with a thickness of 1~10 layer, single-layer graphene with a thickness of
0.33~0.35nm.
Specifically, a part of the photonic crystal fiber 11 is clipped in two single mode optical fibers 12, two coupling units can
Composition waist expansion optical fiber, which is fused, by electric arc slightly bores 13 splicings.At first Coupling point, cladding mode can swash from basic mode
Hair, is then propagated in photonic crystal fiber;At second Coupling point, cladding mode can couple again each other or and basic mode
Then coupling forms interference.The distance between two Coupling points are considered as interfering arm lengths, interference arm lengths, waist length and waist diameter
It is indicated respectively with L, l and d.In the present embodiment, interference arm lengths L, the long l of waist and waist diameter d are respectively 4cm, 400 μm and 179.25 μ
m;Graphene is single-layer graphene, with a thickness of 0.334nm.
Effective refractive index difference between excitation state and excitation state and the phase difference between excitation state and basic mode cause connection
Close interference, the intensity transmission of the sensor can be with is defined as:
Wherein, I1、I2It is the intensity of different mode;It is that mutual modal phase is poor, can indicates are as follows:
Wherein, λ is the wavelength of incident light;ΔneffIt is the difference of the effective refractive index of fibre core and cladding mode;L is two couplings
The distance between point, the physical length corresponding to interferometer.The m rank wavelength X of interferencemIt can indicate are as follows:
When the graphene of cladding submerges target liq, the refractive index of covering occurs in tapered photonic crystal fibre evanescent field
Variation, the difference between core mode and the availability indexes of cladding mode will also change, due in waist expansion optical fiber is slightly bored
The coupling of fibre core and cladding mode and compound, the paddy in corresponding transmitted spectrum is moved.It therefore, can be by measuring corresponding wavelength
It deviates to realize that refractive index detects.
The preparation method of the index sensor of the present embodiment, comprising the following steps:
S1: the composite membrane (PMMA/ of graphene (Graphene) and polymethyl methacrylate (PMMA) is prepared on copper foil
Graphene).Specifically include:
S11: graphene is grown on copper foil (Cu) by chemical vapour deposition technique.
S12: the copper foil with graphene being placed on substrate clean, that surface is smooth, four sides of copper foil are clung with adhesive tape,
So that copper foil is evenly laid out on substrate, it is noted that copper foil is paved when viscous, reduce folding line, it is irregular to be otherwise easy gluing.
In another embodiment, a few drop deionized waters can be dripped on circle/square silicon wafer, and the copper foil with graphene is laid in silicon
On piece presses lightly on copper foil surrounding with tweezers, guarantees that copper foil is fitted closely with silicon wafer, copper foil edge not have the gap, otherwise easily
It flies out.
S13: using sol evenning machine on the copper foil with graphene spin coating polymethyl methacrylate precursor liquid, substrate is put
On objective table, with suction pipe drip it is a few drop mass fractions be 2.5% PMMA solution on copper foil, then first under 500rpm revolving speed
Copper foil after spin coating, is placed on 120 DEG C of bakings on temperature platform by spin coating 3s, then the spin coating 40s under 5000rpm revolving speed
10min keeps PMMA gelling solid to keep enough intensity.The effect of PMMA is support graphene film, be may make after spin coating PMMA
Graphene keeps enough intensity in subsequent processes, is not easy to rupture in the solution.
S2: the composite membrane is transferred to the surface of photonic crystal fiber (PCF) by copper dissolution method.Specifically include:
S21: configuration ferric nitrate etching liquid, wherein the ratio of ferric nitrate and solvent is 15~20g:100ml, and solvent is usually fetched water
Or deionized water 200ml, or use hydrochloric acid (mass fraction for 36~38%), hydrogen peroxide (mass fraction 30%) and go
Ionized water presses the mixed liquor 200ml of 1:1:20 proportional arrangement.
S22: the copper foil after gluing is placed on etching liquid surface, etched corrosion (time is greater than 20min) is pressed from both sides with tweezers
Firmly copper foil drags on rubber gloves by its back side, removes back side graphene, then copper foil is placed on filter paper, is inhaled using filter paper
The liquid at the copper foil back side is received, convenient for shearing copper foil in next step.In another embodiment, the copper foil after gluing is placed on etching liquid table
Face 8min when about 5min, is allowing its back side to drag on rubber gloves, is removing the back side with tweezers clamping copper foil in the process
Graphene, copper foil repeatedly, is then placed on deionized water surface 10min, in the process, continues to scrape by dragging repeatedly, is guaranteed
The graphene of copper foil lower surface is removed clean.
S23: copper foil is placed on hand, and edge adhesive tape is clung and is not coated with graphene, the part for having residue glue and tweezers clamping
Part is cut off, and copper foil is cut into suitable size about 1*1cm according to required size, is clamped with tweezers and is placed on etching liquid surface extremely
Copper foil etching finishes, and obtains the PMMA/ graphene composite film for floating on etching liquid surface.
S24: by hydrochloric acid (mass fraction 36%-38%), hydrogen peroxide (mass fraction 30%) and deionized water according to
The proportional arrangement solution (hydrogen peroxide ratio can be slightly less than 1, reduce bubble) of 1:1:10, reaps this for PMMA/ graphene composite film
In solution, to remove iron nitrate solution bring impurity.The film for not having bubble to adhere to can be fished for glass slide, have bubble to adhere to
Film can be fished for PET sheet, remove bubble removing using the adsorption capacity of PET.PET sheet is clamped with tweezers, and when fishing for, PET tilts certain angle
Composite membrane, can be rushed to culture dish wall, increase the inclination angle of PET, film can be sticked on PET on one side, PET can be proposed water at this time by degree
Then PET is gently put into hydrochloric acid, in dioxygen water mixed liquid by face, PET is withdrawn along the direction perpendicular to film, should not front and back shake
It is dynamic, 2h is impregnated in mixed liquor to remove impurity, then by film transfer into deionized water.Operating process movement will be prevented slowly
Graphene is damaged.
S25: photonic crystal fiber is immersed in deionized water to the bottom end for being placed in composite membrane, then photonic crystal fiber is past
It above mentions, composite membrane is made to be transferred to photonic crystal fiber surface, remove PMMA with acetone again later, pure graphene can be obtained
Film is coated on photonic crystal fiber surface.
The photonic crystal fiber for being coated with graphene film: being placed in 280~320 DEG C of 3.5~4.5h of temperature lower calcination by S3, is increased
Strong film adhesive force obtains graphene optical fiber composite construction.
S4: by optical fiber splicer by the both ends of the graphene optical fiber composite construction respectively with Single-Mode Fiber Coupling, and
It is respectively formed waist expansion optical fiber at two Coupling points slightly to bore, so that index sensor be made.Specifically, optical fiber splicer
Parameter is set as: electric discharge starts intensity+100 for the first time, and electric discharge terminates intensity+100 for the first time, and electric discharge starts intensity+100 again, again
Electric discharge end intensity+100, fritting time+260ms ,+315 μm of advance distance.Wherein, advance distance expression exists two optical fiber
The distance squeezed when arc welding toward centre, slightly to be bored the structure of (bulge), biggish advance distance is available
Biggish waist sizes and shorter taper transitions section length.The waist sizes obtained under the parameter and the taper transitions head of district
Degree are as follows: waist long 400 μm, 179.25 μm of waist diameter, taper transitions section length 4cm.
In above-mentioned steps, preparation and transfer process about PMMA/ graphene composite film can be shown refering to shown in Fig. 2
It is intended to.
The present embodiment additionally provides a kind of system for carrying out refractive index detection using above-mentioned index sensor, such as Fig. 5 institute
Show comprising index sensor 10, light source 20, sample room 30 and signal processing system 40, the index sensor 10 are set
In in the sample room 30, both ends are connect with the light source 20 and the signal processing system 40 respectively.
Specifically, the light source 10 uses amplified spontaneous emission source (ASE), the signal processing system 40 is using light source point
Analyzer (OSA, Yokogawa AQ6370D), sample room 30 can be cuvette or collection airbag, be respectively used to dress various concentration
Fluid sample and gaseous sample, as refractometry sample, transmission spectrum of the sensor under different refractivity by amplification from
Send out radiation source and spectroanalysis instrument detection.
Surface topography and molecular structure characterization
Using scanning electron microscope (SEM, TESCAN MIRA3) and Raman spectrum (LabRAM HR Evolution,
HORIBA Scientific) to the surface topography of graphene optical fiber composite construction made from above-described embodiment and molecular structure into
Characterization is gone.As shown in Fig. 3 (a), SMF splices in the end of PCF, and in fusion process, the PCF stomata of end perimeter collapses completely
It falls into, then, heat sealing machine can control motor and accurately push middle section between SMF and PCF, and form the widened cone of waist
Shape.Shown in outer surface pattern such as Fig. 3 (b) of taper PCF, it is seen that outer surface is uniform, shows that graphene film is equal in the distribution of the surface PCF
It is even.Raman spectrum is as shown in Figure 4, it is seen that G (~1591cm-1) and 2D (~2697cm-1) peak and graphene normalized Raman peak one
It causing, it was demonstrated that the film that PCF is coated is made of graphene really, meanwhile, the relative intensity ratio at the peak G and 2D illustrates graphite less than 1
Alkene film is single layer structure.
Detect sucrose solution
Use the sucrose solution with various concentration (0~233ppm) as the refractive index liquid sample for being used for refractometry
Product, their refractive index are detected at room temperature 300K from 1.3338 to 1.3376, by sensor.
In order to study influence of the graphene for sucrose solution concentration, following control experiment has been carried out: manufacture comparison optical fiber
Sensor, it is substantially the same manner as Example 1, the difference is that, the surface PCF does not have coated graphite alkene layer.Utilize the comparison light
Fiber sensor detects the maximum offset of the sucrose solution of 0ppm and 230ppm, shown in experimental result such as Fig. 6 (a), two concentration
Wave length shift between (0ppm and 230ppm) is only 0.3nm.And it is different to utilize the index sensor of above-described embodiment to detect
The maximum offset of the sucrose solution of concentration, shown in experimental result such as Fig. 6 (b), between two concentration (0ppm and 230ppm)
Wave length shift can achieve 1nm.It can be seen that graphene film can significantly improve the sensitivity of index sensor.
Meanwhile with the increase of sucrose concentration, trough is mobile to shorter wavelength, the reason is as follows that: when contact with sucrose graphite
When alkene sensing layer, the effective refractive index of covering be will increase, but the refractive index of fibre core is constant, therefore, difference (Δ neff) refractive index
It is reducing, thus, according to formula (3), wavelength reduces, and shows the increase with sucrose concentration, the output transmission spectrum of refractometer
Blue shift will occur.Experimental result and notional result are coincide very much.The value of trough wavelength and concentration is fitted by linear regression model (LRM),
As a result as shown in Figure 6, the results showed that, the coefficient R of calibration curve2It is 0.98233, in given sucrose solution concentration range
Interior, index sensor shows fairly good linear response, and graphene is 3.36pm/ppm to the sensibility of sucrose solution.Altogether
The variation relation to shake between the wavelength shift at peak and the refractive index of external solution is as shown in Figure 7, wherein discrete point is actual measurement
Point, straight line are linear fit curve (R'2=0.98217), the experimental results showed that, when the external refractive index is changed to from 1.3338
When 1.3376, the sensitivity of sensor can achieve 205.26nm/RIU.
Detect hydrogen sulfide gas
The index sensor of embodiment 1 is not merely confined to the experiment of sucrose solution, such as glucose, and sodium chloride etc. is molten
Liquid can be carried out testing, and if depositing one layer of other sensitive materials on graphene film surface, can be used to examine
Survey other solution or gas.In this experiment, nanometer is deposited on the graphene film surface of the index sensor of embodiment 1
Copper, for detecting hydrogen sulfide gas.
0ppm, 10ppm, 20ppm, 40ppm, 60ppm, this seven kinds of concentration of 70ppm, 80ppm are respectively configured using collection airbag
Hydrogen sulfide gas and tested, obtain spectrogram as shown in Figure 8.It can be seen that with the increase of sulfureted hydrogen gas concentration, light
Blue-shifted phenomenon has occurred in the monitoring trough of spectrum.The reason is that: the hydrogen sulfide in the Nanometer Copper adsorbed gas on graphene film surface
After molecule, itself refractive index will change, and the cladding-effective-index of photonic crystal fiber is made to change, and cause photon brilliant
The optical path difference of fibre core and covering changes in body optical fiber, therefore can be from the interference wave observed in transmitted spectrum on spectrometer
Paddy will shift, so that the offset of the concentration of gas and wavelength be connected, achieve the purpose that detection gas concentration.
The experimental results showed that the index sensor of embodiment 1 sulfureted hydrogen gas concentration be 0~80ppm within the scope of be in
Existing good linear response, as shown in Figure 9.Wherein, discrete point is actual spot of measurement, and straight line is linear fitting curve, it is seen that its
High (the R of the linearity2It=0.9909) is, and to the sensitivity of hydrogen sulfide gas 8.5pm/ppm.The sensor is easily fabricated, at
This is low, small in size, can be used for the detection of low concentration hydrogen sulphide gas.
Compared with the existing technology, the index sensor of the utility model is based on graphene coated optical fiber and has waist
Expand double thick wimble structures of optical fiber as interferometer, is combined by optical fiber with graphene, using the special construction of graphene to molten
Molecule in liquid has adsorptivity, thus changes the refractive index of optical fiber, improves its sensitivity;Expand double optical fiber using waist slightly to bore
The coupling of structure progress fibre core and cladding mode and compound, realization multiple-mode interfence.The index sensor of the utility model is for object
Matter concentration (such as hydrogen sulfide gas, sucrose) detection has High Linear response and excellent sensitivity, and has at low cost, production side
The feature that method is simple, repeatability is high, can mass production use.
Above-described embodiments merely represent several embodiments of the utility model, the description thereof is more specific and detailed,
But it cannot be understood as the limitations to utility model patent range.It should be pointed out that for the common skill of this field
For art personnel, without departing from the concept of the premise utility, various modifications and improvements can be made, these are belonged to
The protection scope of the utility model.
Claims (8)
1. a kind of index sensor, it is characterised in that: including a photonic crystal fiber and two single mode optical fibers, the photonic crystal
The both ends of optical fiber with a Single-Mode Fiber Coupling, and are respectively formed at two Coupling points a waist and expand optical fiber and slightly bore respectively;
The photonic crystal fiber surface is coated with graphene layer.
2. index sensor according to claim 1, it is characterised in that: the distance between described two Coupling point is 3.9
~4.1cm.
3. index sensor according to claim 2, it is characterised in that: it is a length of that the waist expands the waist that optical fiber is slightly bored
395~405 μm, waist diameter is 179~180 μm.
4. index sensor according to claim 3, it is characterised in that: the distance between described two Coupling point is 4cm;
The waist expands a length of 400 μm of waist that optical fiber is slightly bored, and waist diameter is 179.25 μm.
5. index sensor according to claim 1, it is characterised in that: the graphene layer is 1~10 layer of graphene.
6. index sensor according to claim 5, it is characterised in that: the graphene layer is single-layer graphene, thick
Degree is 0.33~0.35nm.
7. a kind of refractive index detection system, it is characterised in that: including the index sensor any in claim 1~6,
Light source, sample room and signal processing system, the index sensor be set to the sample room in, both ends respectively with the light
Source is connected with the signal processing system.
8. refractive index detection system according to claim 7, it is characterised in that: the signal processing system is spectrum analysis
Instrument.
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