CN106290250A - Optical-fiber type that modified graphene strengthens is poisonous/harmful gas sensor and preparation method thereof - Google Patents
Optical-fiber type that modified graphene strengthens is poisonous/harmful gas sensor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses the optical-fiber type that a kind of modified graphene strengthens poisonous/harmful gas sensor and preparation method thereof, this modified graphene strengthen optical-fiber type poisonous/harmful gas sensor, including the light source being sequentially connected with, input optical fibre, modular converter, sensing module, output optical fibre and spectrogrph;Modular converter is few mould LPFG mode conversion module, for by LP in incident illumination01The energy of basic mode transfers to LP02In high-order mode;The core of sensing module is few mould long-period gratings, and its top layer is modified graphene layer;Modified graphene layer is the Graphene mixed with impurity element, and impurity element can improve Graphene to CH4Or CO or NH3Adsorption rate.Optical-fiber type that this modified graphene strengthens is poisonous/and harmful gas sensor can monitor the harmful gass such as methane, carbon monoxide or ammonia fast and accurately, and concentration can be detected;Preparation method is simple.
Description
Technical field
The present invention relates to optical fiber sensing detection technology field, relate in particular to the optical-fiber type that a kind of modified graphene strengthens
Poisonous/harmful gas sensor and preparation method thereof.
Background technology
In recent years, global atmosphere problem of environmental pollution is day by day serious, and in air, the detection of every gas componant index is gradually
Become emphasis of concern.Gas (CH4) be a kind of colorless and odorless gas, deposit under mine, when gas density 5~
16% and oxygen concentration more than 12% time, meeting naked light will explode, so the accurately detection of gas density can be coalman people
Safety guarantee is provided;Winter, China's part mountain area and rural area are by heating of lighting stove, and the family in city also can use coal gas, sky
So gas etc., if imperfect combustion, can cause carbon monoxide (CO) to be poisoned, and threaten people's life security;Ammonia can be used for manufacturing nitrogen
Fertilizer, compound fertilizer, nitric acid etc., be widely used in the industries such as chemical industry, light industry, chemical fertilizer, pharmacy, as Ammonia in Air gas (NH3) concentration
Time too high, respiratory system and the skin of also calcination people can be stimulated, be detrimental to health.For these poisonous/harmful chemicals gas
Carry out the detection of safety the most again, have important research and Practical significance in sensing detection field.
Fiber-optic grating sensor, as a kind of fiber optic passive device, does not has circuit discharging dangerous, has that volume is little simultaneously, becomes
This is the lowest, electromagnetism interference, the advantage such as can imbed, be particularly suitable under the high-risk environment such as colliery, chemical industry, nuclear power to poisonous/
Harmful and flammable explosive gas detects.
The length that fiber-optic grating sensor presses screen periods is different, can be divided into short period optical fiber grating, also known as optical fiber Bradley
Lattice grating, FBG, and LPFG, LPFG.Existing FBG part to temperature, strain, the variable quantity that vibrates all
The most sensitive, but variablees such as being enclosed in the refractive index of fiber grating ambient substance, acid-base value, concentration is but lacked sensitivity,
Therefore, the application in the field such as biology, chemistry, environment is restricted.And LPFG, LPFG, sensor is due to it
The difference of sensor mechanism, has higher susceptiveness at aspects such as measuring the refractive index of external substance, acid-base value, concentration.Therefore, exist
Chemical gas and the sensing of liquid and context of detection, use long-period fiber grating sensor to carry out Fibre Optical Sensor research mostly.
Major part LPFG gas sensor is all write grating in single-mode fiber the most both at home and abroad, applies erosion simultaneously
Carve, cut and wrap up in the means such as deposited to realize gas sensing.2010, China Mining University, by observing the change of luminous power, was visited
Measure the CH of 5% gas concentration4.2011, Remmel et al. covered nanocrystal copper doped on LPFG
Zirconia film material, detected the CO concentration of 4ppmv.Within 2007, the TaiWan, China National Defence University is at the fiber grating etched
Upper covering polyaniline medium, to NH3Detection sensitivity reached 0.073pm/ppm.But limited by single-mode fiber structure, fine
In core basic mode energy, the mode of energy for heat transfer agent is inefficient, and therefore the sensitivity of the gas sensor of single-mode fiber is relatively
Low.Although people are many improvement in order to the sensitivity improving fiber-optic grating sensor did, as carried out the covering of fiber grating
Etching thinning, to use high index of refraction organic polymer thin film or nano material covers LPFG surface etc., these methods are each
Long, but all cannot change the optical fiber structure essence to sensitivity limit.
Summary of the invention
In order to solve above-mentioned technical problem, poisonous/harmful gas of optical-fiber type that the present invention provides a kind of modified graphene to strengthen
Body sensor and preparation method thereof, this modified graphene strengthen optical-fiber type poisonous/harmful gas sensor can be fast and accurately
Monitor the harmful gass such as methane, carbon monoxide or ammonia, and concentration can be detected.
To this end, technical scheme is as follows:
A kind of modified graphene strengthen optical-fiber type poisonous/harmful gas sensor, including the light source being sequentially connected with, input
Optical fiber, sensing module, output optical fibre and spectrogrph;Also include modular converter;Described modular converter is few mould long period optical fiber light
Grid mode conversion module, for by LP in incident illumination01The energy of basic mode transfers to LP02In high-order mode;Described sensing module
Core is few mould long-period gratings, and its top layer is modified graphene layer;Described modified graphene layer is the stone mixed with impurity element
Ink alkene, described impurity element can improve Graphene to CH4Or CO or NH3Adsorption rate.
A kind of modified graphene strengthen optical-fiber type poisonous/harmful gas sensor, including light source, bonder, input light
Fibre, sensing module, output optical fibre, spectrogrph and modular converter;Described modular converter turns for few mould LPFG pattern
Die change block, for by LP in incident illumination01The energy of basic mode transfers to LP02In high-order mode;The core of described sensing module is few mould
Long-period gratings, its top layer is modified graphene layer;Described modified graphene layer is the Graphene mixed with impurity element, described miscellaneous
Prime element can improve Graphene to CH4Or CO or NH3Adsorption rate;Three ports of described bonder respectively with described light source, biography
Sense module is connected with spectrogrph;Described modular converter is connected with described sensing module, and the free end of described sensing module is coated with
One layer of silverskin.Light source enters modular converter through bonder, by LP in incident illumination01The energy of basic mode transfers to LP02In high-order mode,
Then LP02Light in high-order mode enters sensing module, CH in detection environmental gas4Or CO or NH3Content;Then light is through silverskin
Reflection is from backtracking to bonder, and its data carried show through spectrogrph.
Preferably, described impurity element is Si, Al, Fe, Co, Ni, Ru, Pt, N, B, Si or Al.Research shows, at Graphene
Middle doping N, B or Al element can improve graphenic surface CH very well4Absorbability, doping Si, Al, VIII B (Fe, Co, Ni,
Ru, Pt) adsorption function of CO gas can be improved very well, doping B, Si or Al can strengthen NH3Energy of adsorption.
Further, the preparation method of described sensing module, comprise the steps:
1) in less fundamental mode optical fibre, write the long-period gratings between 300~600 μm, obtain the few mould with long-period gratings
Fiber grating;
2) the described less fundamental mode optical fibre two ends with long-period gratings are fixed between two rotary shafts of uniform rotation, make
The surface of this less fundamental mode optical fibre is performed etching, then utilizes in alkali liquor and Fluohydric acid., water with hydrofluoric acid solution plane tangent by it
Wash, be dried, make cladding thickness be reduced to 18~40 μm;
Or the described less fundamental mode optical fibre with long-period gratings is carried out side cut, makes cladding thickness be reduced to 18~40
μm;
3) by the graphene coated doped with impurity element through step 2) process after optical fiber surface, obtain described sensing
Module.This graphene uniform, regular is deposited on few mould long-period gratings optical fiber that cladding thickness is thinning, preferably controls stone
The thickness that thickness is single-layer graphene of ink alkene layer.
Few mould LPFG mode conversion module and LPFG surface that the present invention is exclusive etch, wrap up in
The measure of applying, can increase substantially the sensitivity of LPFG gas sensor, be expected to put forward detection limit from ppm magnitude
High to ppb magnitude.Meanwhile, the modified graphene material covered with the less fundamental mode optical fibre surface of long-period gratings in the present invention is logical
The specific trace impurity of overdoping or group, can be greatly improved the absorption power of test to certain specific gas.Therefore, by design
Adulterate specific impurity or group and ratio thereof, the sensing detection to one or more poisonous/harmful gas single can be realized.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme is described in detail.
Embodiment 1
A kind of modified graphene strengthen optical-fiber type poisonous/harmful gas sensor, including the light source being sequentially connected with, input
Optical fiber, modular converter, sensing module, output optical fibre and spectrogrph;Modular converter is few mould LPFG patten transformation
Module, for by LP in incident illumination01The energy of basic mode transfers to LP02In high-order mode;The core of sensing module is few mould long period
Grating, its top layer is modified graphene layer;Modified graphene layer is the Graphene mixed with impurity element, and impurity element can improve stone
Ink alkene is to CH4Or CO or NH3Adsorption rate.For being used for detecting CH4Sensor, select doped with the graphite of N, B or Al element
Alkene is as modified graphene layer;
For the sensor for detecting CO, select doped with Si, Al or VIII B (Fe, Co, Ni, Ru, Pt) element
Graphene is as modified graphene layer;
For being used for detecting NH3Sensor, select doped with the Graphene of B, Si or Al as modified graphene layer;
In the present embodiment, the preparation method of sensing module, comprises the steps:
1) in less fundamental mode optical fibre, write the long-period gratings between 300~600 μm, obtain the few mould with long-period gratings
Optical fiber;
2) the less fundamental mode optical fibre two ends with long-period gratings are fixed between two rotary shafts of uniform rotation so that it is with
Hydrofluoric acid solution plane tangent, performs etching the surface of this less fundamental mode optical fibre, then utilizes in alkali liquor and Fluohydric acid., washing, dry
Dry, make cladding thickness be reduced to 18~40 μm;
Or the less fundamental mode optical fibre with long-period gratings is carried out side cut, make cladding thickness be maintained at be reduced to 18~
40μm;
3) by the graphene coated mixed with impurity element through step 2) process after optical fiber surface, obtain sensing module.
This graphene uniform, regular is deposited on few mould long-period gratings optical fiber that cladding thickness is thinning.
Embodiment 2
A kind of modified graphene strengthen optical-fiber type poisonous/harmful gas sensor, including light source, bonder, input light
Fibre, sensing module, output optical fibre, spectrogrph and modular converter;Modular converter is few mould LPFG patten transformation mould
Block, for by LP in incident illumination01The energy of basic mode transfers to LP02In high-order mode;The core of sensing module is few mould long period light
Grid, its top layer is modified graphene layer;Modified graphene layer is the Graphene mixed with impurity element, and impurity element can improve graphite
Alkene is to CH4Or CO or NH3Adsorption rate;Three ports of bonder are connected with light source, sensing module and spectrogrph respectively;Conversion
Module is connected with sensing module, and the free end of sensing module is coated with one layer of silverskin.Light source enters modular converter through bonder,
By LP in incident illumination01The energy of basic mode transfers to LP02In high-order mode, then LP02Light in high-order mode enters sensing module, inspection
Survey CH in environmental gas4Or CO or NH3Content;Then light reflects from backtracking to bonder through silverskin, its data carried
Show through spectrogrph.Integrated composition saves space.
For being used for detecting CH in the present embodiment4Sensor, select doped with the Graphene of N, B or Al element as changing
Property graphene layer;
For the sensor for detecting CO, select doped with Si, Al or VIII B (Fe, Co, Ni, Ru, Pt) element
Graphene is as modified graphene layer;
For being used for detecting NH3Sensor, select doped with the Graphene of B, Si or Al as modified graphene layer;
In the present embodiment, the preparation method of sensing module, comprises the steps:
1) in less fundamental mode optical fibre, write the long-period gratings between 300~600 μm, obtain the few mould with long-period gratings
Optical fiber;
2) the less fundamental mode optical fibre two ends with long-period gratings are fixed between two rotary shafts of uniform rotation so that it is with
Hydrofluoric acid solution plane tangent, performs etching the surface of this less fundamental mode optical fibre, then utilizes in alkali liquor and Fluohydric acid., washing, dry
Dry, make cladding thickness be reduced to 18~40 μm;
Or the less fundamental mode optical fibre with long-period gratings is carried out side cut, makes cladding thickness be reduced to 18~40 μm;
3) by the graphene coated doped with impurity through step 2) process after optical fiber surface, and the most silver-plated film,
Obtain described sensing module.This graphene uniform, regular is deposited on few mould long-period gratings optical fiber that cladding thickness is thinning
On.
Specifically, in the present embodiment, modular converter is one is the less fundamental mode optical fibre of 430 μm at fibre core write screen periods,
Being the fibre core of a diameter of 19.0 μm centered by its structure, outside is the covering of a diameter of 125 μm, has allowed LP in fibre core01、
LP11、LP21、LP02Four line polarized light field mode transmission, then allow the light field mode of hundreds of higher order to transmit in covering.?
In mode conversion module, due to long-period gratings Λ1Existence, it is possible to obtain LP01With LP02The phase place of two core mode
Join, thus by LP in incident illumination01The energy of basic mode transfers to LP02In high-order mode;Sensing module lacks with identical with modular converter
Mode fiber is made, and except for the difference that the screen periods in fibre core write is Λ2, its covering is thinning through chemical attack or side cut
After, wrapping one layer of modified graphene material the most regularly, equably, the function of this module is to make the LP into shining02Mould
Realize coupled resonance with the low step mode of the onwards transmission in covering, and gradually develop during onwards transmission and decay,
The variations in refractive index of extraneous test substance can affect its effective refractive index and resonant wavelength, thus can perception and detection external substance
The change of refractive index.Finally, by the effect of silverskin, the energy of emergent light can be transferred back to LP01In basic mode, and from incidence end
Output energy.
The physical mechanism of two module work is all conversion and the coupling principle of pattern in fibre-optic waveguide, first by incident illumination
The cycle of being input to is Λ1It is in few mould LPFG of 430 μm, makes basic mode LP01Energy transfer to high-order mode LP02
On, it is then Λ by the cycle2, to have passed through etching thinning and wrap few mould LPFG of modified graphene material,
Make LP02In mould and covering, the low step mode of transmission meets phase-matching condition and realizes coupled resonance, when the test substance of surrounding
During variations in refractive index, the minimum order mode in fibre cladding mould is the most all absorbed in cover layer above, its effective folding
The rate of penetrating becomes close to surface coating, leaves the blank that the effective refractive index of cladding mode is distributed, meanwhile, all high-orders
The effective refractive index of cladding mode moves to recover the distribution of original effective refractive index, this is moved through LPFG
The phase-matching condition that the attenuation band of each resonance wavelength of transmission spectrum moves to more low order reflects, and i.e. rolls over along with the external world
Penetrating the change of rate, the resonance wavelength of transmission spectrum can be drifted about, and then the variations in refractive index demodulating test substance is floated with wavelength
The corresponding relation moved, it is achieved the high accuracy of material, highly sensitive sensing measurement to external world.
Claims (5)
1. modified graphene strengthen optical-fiber type poisonous/harmful gas sensor, including the light source being sequentially connected with, input light
Fibre, sensing module, output optical fibre and spectrogrph;It is characterized in that: also include modular converter;Described modular converter is few mould length week
Phase fiber grating mode conversion module, for by LP in incident illumination01The energy of basic mode transfers to LP02In high-order mode;Described sensing
The core of module is few mould long-period gratings, and its top layer is modified graphene layer;Described modified graphene layer is mixed with impurity unit
The Graphene of element, described impurity element can improve Graphene to CH4Or CO or NH3Adsorption rate.
2. a modified graphene strengthens optical-fiber type is poisonous/harmful gas sensor, it is characterised in that: include light source, coupling
Device, input optical fibre, sensing module, output optical fibre, spectrogrph and modular converter;Described modular converter is few mould long period optical fiber light
Grid mode conversion module, for by LP in incident illumination01The energy of basic mode transfers to LP02In high-order mode;The core of described sensing module
Portion is few mould long-period gratings, and its top layer is modified graphene layer;Described modified graphene layer is the graphite mixed with impurity element
Alkene, described impurity element can improve Graphene to CH4Or CO or NH3Adsorption rate;Three ports of described bonder respectively with institute
State light source, sensing module is connected with spectrogrph;Described modular converter is connected with described sensing module, and described sensing module
Free end is coated with one layer of silverskin.
3. as claimed in claim 1 or 2 modified graphene strengthens optical-fiber type is poisonous/harmful gas sensor, it is characterised in that:
Described impurity element is Si, Al, Fe, Co, Ni, Ru, Pt, N, B, Si or Al.
4. as claimed in claim 1 modified graphene strengthens optical-fiber type is poisonous/harmful gas sensor described in sensing module
Preparation method, it is characterised in that comprise the steps:
1) in less fundamental mode optical fibre, write the long-period gratings between 300~600 μm, obtain the less fundamental mode optical fibre with long-period gratings
Grating;
2) the described less fundamental mode optical fibre two ends with long-period gratings are fixed between two rotary shafts of uniform rotation so that it is with
Hydrofluoric acid solution plane tangent, performs etching the surface of this less fundamental mode optical fibre, then utilizes in alkali liquor and Fluohydric acid., washing, dry
Dry, make cladding thickness be reduced to 18~40 μm;
Or the described less fundamental mode optical fibre with long-period gratings is carried out side cut, makes cladding thickness be reduced to 18~40 μm;
3) by the graphene coated mixed with impurity element through step 2) process after optical fiber surface, obtain described sensing module.
5. as claimed in claim 2 modified graphene strengthens optical-fiber type is poisonous/harmful gas sensor described in sensing module
Preparation method, it is characterised in that comprise the steps:
1) in less fundamental mode optical fibre, write the long-period gratings between 300~600 μm, obtain the less fundamental mode optical fibre with long-period gratings
Grating;
2) the described less fundamental mode optical fibre two ends with long-period gratings are fixed between two rotary shafts of uniform rotation so that it is with
Hydrofluoric acid solution plane tangent, performs etching the surface of this less fundamental mode optical fibre, then utilizes in alkali liquor and Fluohydric acid., washing, dry
Dry, make cladding thickness be reduced to 18~40 μm;
Or the described less fundamental mode optical fibre with long-period gratings is carried out side cut, makes cladding thickness be reduced to 18~40 μm;
3) by the graphene coated mixed with impurity element through step 2) process after optical fiber surface, and the most silver-plated film,
To described sensing module.
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CN107831195A (en) * | 2017-10-30 | 2018-03-23 | 上海应用技术大学 | A kind of animal flesh metal doping nano graphene olfactory sensor |
CN108226054A (en) * | 2018-01-02 | 2018-06-29 | 重庆理工大学 | The production method of overlay film optical fiber carbon monoxide transducer and its detection method of sensor and carbonomonoxide concentration |
CN110186875A (en) * | 2019-05-21 | 2019-08-30 | 天津大学 | Surface plasmon resonance optical-fiber type pH value measurement method and sensor |
CN113189048A (en) * | 2021-04-27 | 2021-07-30 | 武汉理工大学 | Long-period fiber grating NH3 gas sensor based on graphene oxide/cellulose acetate |
CN115642465A (en) * | 2022-12-23 | 2023-01-24 | 中国科学院长春光学精密机械与物理研究所 | Fundamental mode conversion system based on non-mode selection photon lantern |
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CN107831195A (en) * | 2017-10-30 | 2018-03-23 | 上海应用技术大学 | A kind of animal flesh metal doping nano graphene olfactory sensor |
CN108226054A (en) * | 2018-01-02 | 2018-06-29 | 重庆理工大学 | The production method of overlay film optical fiber carbon monoxide transducer and its detection method of sensor and carbonomonoxide concentration |
CN108226054B (en) * | 2018-01-02 | 2020-08-18 | 重庆理工大学 | Method for manufacturing coated optical fiber carbon monoxide sensor, sensor thereof and method for detecting carbon monoxide concentration |
CN110186875A (en) * | 2019-05-21 | 2019-08-30 | 天津大学 | Surface plasmon resonance optical-fiber type pH value measurement method and sensor |
CN113189048A (en) * | 2021-04-27 | 2021-07-30 | 武汉理工大学 | Long-period fiber grating NH3 gas sensor based on graphene oxide/cellulose acetate |
CN115642465A (en) * | 2022-12-23 | 2023-01-24 | 中国科学院长春光学精密机械与物理研究所 | Fundamental mode conversion system based on non-mode selection photon lantern |
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Application publication date: 20170104 |