CN108387494A - A kind of PM based on hollow Bragg optical fiber2.5Concentration detection apparatus - Google Patents
A kind of PM based on hollow Bragg optical fiber2.5Concentration detection apparatus Download PDFInfo
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- CN108387494A CN108387494A CN201810174701.5A CN201810174701A CN108387494A CN 108387494 A CN108387494 A CN 108387494A CN 201810174701 A CN201810174701 A CN 201810174701A CN 108387494 A CN108387494 A CN 108387494A
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- optical fiber
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- bragg optical
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- iodine
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- 238000001514 detection method Methods 0.000 title claims abstract description 26
- 230000003287 optical effect Effects 0.000 title description 8
- 239000013307 optical fiber Substances 0.000 claims abstract description 127
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229920001197 polyacetylene Polymers 0.000 claims abstract description 39
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 35
- 239000011630 iodine Substances 0.000 claims abstract description 35
- 239000000835 fiber Substances 0.000 claims abstract description 34
- 239000010409 thin film Substances 0.000 claims abstract description 22
- 238000012360 testing method Methods 0.000 claims abstract description 20
- 239000003463 adsorbent Substances 0.000 claims abstract description 11
- 239000010408 film Substances 0.000 claims description 35
- 239000007789 gas Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 12
- 239000003792 electrolyte Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 229910052709 silver Inorganic materials 0.000 claims description 9
- 239000004332 silver Substances 0.000 claims description 9
- 206010070834 Sensitisation Diseases 0.000 claims description 8
- 230000008313 sensitization Effects 0.000 claims description 8
- 229910001868 water Inorganic materials 0.000 claims description 8
- 229920001971 elastomer Polymers 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000003213 activating effect Effects 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 229910052763 palladium Inorganic materials 0.000 claims description 6
- 230000001235 sensitizing effect Effects 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 230000005518 electrochemistry Effects 0.000 claims description 4
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 3
- 230000002572 peristaltic effect Effects 0.000 claims description 3
- 230000005855 radiation Effects 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 239000010410 layer Substances 0.000 claims 13
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 239000012792 core layer Substances 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 235000011150 stannous chloride Nutrition 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 13
- 239000002245 particle Substances 0.000 abstract description 13
- 230000035945 sensitivity Effects 0.000 abstract description 9
- 230000033001 locomotion Effects 0.000 description 14
- 238000000034 method Methods 0.000 description 13
- 238000000411 transmission spectrum Methods 0.000 description 13
- 238000012417 linear regression Methods 0.000 description 9
- 239000010419 fine particle Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 230000004044 response Effects 0.000 description 7
- 239000012528 membrane Substances 0.000 description 6
- 239000013618 particulate matter Substances 0.000 description 6
- 239000000443 aerosol Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 4
- 229920000128 polypyrrole Polymers 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000000149 argon plasma sintering Methods 0.000 description 3
- 230000005250 beta ray Effects 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000002121 nanofiber Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000003915 air pollution Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 150000001345 alkine derivatives Chemical class 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 230000002463 transducing effect Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
- G01N15/075—Investigating concentration of particle suspensions by optical means
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/08—Optical fibres; light guides
- G01N2201/088—Using a sensor fibre
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Dispersion Chemistry (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a kind of PM based on hollow Bragg optical fiber2.5Concentration detection apparatus, including superradiance wideband light source SLD, optical fiber PM2.5Concentration sensor, test gas chamber, PM2.5Generator, controlled valve, gas flowmeter, spectroanalysis instrument and the computer being connect with spectroanalysis instrument, optical fiber PM2.5Concentration sensor is made of single mode optical fiber, air-core inner surface coated with hollow Bragg optical fiber, multimode fibre and the optical fiber connector for mixing the photic conductive adsorbent thin film of iodine polyacetylene.The present invention is coated in the air-core inner surface of hollow Bragg optical fiber to PM2.5Particle mixes iodine polyacetylene nano thin-film with photic conductive suction-operated, can give full play to the suction-operated of sensor, the PM based on this formation2.5Concentration sensor, show high sensitivity, it is simple in structure the features such as.
Description
Technical field
The present invention relates to technical field of optical fiber sensing, and in particular to a kind of hollow Bragg based on film refractive index variation
Optical fiber fine particle concentration detection apparatus.
Background technology
Airborne fine particulate matter PM2.5It is the primary pollutant of air pollution, PM2.5It is that aerodynamic diameter is less than or equal to
2.5 microns of particulate matter.PM in air2.5Main source have：Fire coal, sulfate, nitrate and organic matter etc..PM2.5To people
Body health, daily life and atmosphere quality cause tremendous influence.Therefore, to airborne fine particulate matter PM2.5Mass concentration
It is detected, for reducing prevalence, ensures that life security, the generation of air pollution preventing have highly important meaning
Justice.
Currently used for fine particle PM in air2.5The detection method of mass concentration mainly has gravimetric method, β ray attenuation methods
And light scattering method etc..Wherein, gravimetric method is by particle sampler by the particle sampling to sampler in air, so
It is tested gas afterwards and enters PM2.5Cutter, the particle by diameter more than 2.5 microns detach, and diameter is less than or equal to 2.5 microns
Particle is delayed on the filter membrane of constant weight with air-flow through separator outlet.According to the weight difference of filter membrane before and after sampling and adopt
The volume of sample, calculates PM2.5Mass concentration.But the accuracy of this method is substantially dependent upon sampling flow and analysis institute
The uncertainty of balance error, and exist and be unable to real-time online measuring, cumbersome, the shortcomings of sampler is heavy.β rays
The operation principle of damped method is that surrounding air is sucked by sampler, and by being discharged after cutter and filter membrane, diameter is less than or equal to
2.5 microns of particulate matter is deposited on above filter membrane, when β rays when the filter membrane that deposits particulate matter by that can occur declining for energy
Subtract, PM is found out by the measurement to β ray attenuation amounts2.5Mass concentration.But the accuracy that β ray attenuation methods measure is not only
It is related with the sampling flow of sampler, it is also influenced by particulate component, and easily influenced by outside environmental elements.Light scattering method
Mie (Michaelis) scatterings are based primarily upon, light source sends out light beam directive gas channel, and light scatters on particulate matter, and directive is each
A direction, the light intensity difference received by a certain solid angle in a certain direction can find out PM2.5Mass concentration.Light scattering
Method measuring speed is fast, and accuracy is high, energy on-line checking, but this optical system is complex.
Fibre optical sensor is a kind of small, and corrosion-resistant, it can be achieved that remote monitor on-line for a long time, sensing unit structures are simple
It is single, it is reliable and stable, easily form the optical type fine particle PM of optical fiber sensing network2.5Sensor.
In the optical fiber fine particle PM modulated based on spectral intensity2.5In terms of sensor research, the seedling heart to it is equal (light laser with
The particle beams, 2014,26 (11):216-219.) according to the strong constraint energy of micro-nano fiber and big evanscent field the characteristics of, utilize micro-nano
A kind of the characteristics of causing added losses after optical fiber surface absorption aerosol particle, it is proposed that confined air based on micro-nano fiber sensing
Between aerosol detection method, sensing device mainly by semiconductor laser (1550nm), a diameter of 1.5 μm of micro-nano fiber pass
Sensor, detector and computer composition, aerosol sensing process have higher requirement to light source stability.Hongyi Qin etc.
(Journal of Aerosol Science, 2012,45,19~25.) proposes that a kind of gas based on polypyrrole nano thin-film is molten
Glue Fibre Optical Sensor scheme coats polypyrrole nano thin-film, particulate and polypyrrole nanometer on the optical fiber connector polished
The photic electrostatic interaction of film, to change the optical property of polypyrrole nano thin-film, when the incident light of optical fiber is by film reflector,
Detector can detect the variable quantity of reflection signal light intensity, you can obtain aerosol concentration.It is with small, operation letter
It is single, detection cost is effectively reduced, but this method, to the uniformity of coat, smooth degree has higher requirements, and sense
Signal belongs to intensity modulated, is easily influenced by ambient temperature and humidity fluctuation etc..
Invention content
Present invention aims at, give full play to mix iodine polyacetylene nano thin-film to thin for overcome the deficiencies in the prior art
Grain object (PM2.5) photic conductive suction-operated, hollow Bragg optical fiber high sensitivity, fibre core be larger, fast response time, wavelength tune
A kind of the features such as system and refractive index are sensitive, it is proposed that PM based on hollow Bragg optical fiber2.5Concentration detection apparatus, with realization pair
PM2.5The high sensitivity of concentration, high stability detection.
The present invention is based on the PM of hollow Bragg optical fiber2.5Concentration detection apparatus, including superradiance wideband light source SLD, optical fiber
PM2.5Concentration sensor tests gas chamber, PM2.5Generator, controlled valve, gas flowmeter, spectroanalysis instrument and and spectrum analysis
The computer of instrument connection；
The optical fiber PM2.5Concentration sensor is coated with by a single mode optical fiber, an air-core inner surface and is mixed the poly- second of iodine
Hollow Bragg optical fiber, a multimode fibre and the two optical fiber connector compositions of the photic conductive adsorbent thin film of alkynes, single-mode optics
Fine output end is connect by optical fiber connector with the input terminal of hollow Bragg optical fiber, and the output end of hollow Bragg optical fiber passes through
The input terminal of optical fiber connector and multimode fibre connects；
The hollow Bragg optical fiber is by a diameter of 200 μm of air-core, the one-dimensional photon being enclosed in outside air-core
Crystal layer, the covering being enclosed in outside 1-D photon crystal layer are constituted；The 1-D photon crystal layer is by periodical cross-distribution
High refractive index layer and low-index layer composition, the refractive index of each high refractive index layer is identical with thickness, the refraction of each low-index layer
Rate and thickness are also identical, and the transmission wave band centre wavelength of hollow Bragg optical fiber is at 1.55 μm；
The optical fiber PM2.5Concentration sensor is set in test gas chamber, and air inlet is provided on the test gas chamber and is gone out
Gas port, the air inlet by controlled valve respectively with PM2.5Generator is connected with the gas flowmeter of control nitrogen flow；Institute
The both ends open end for stating hollow Bragg optical fiber is directly communicated with the test indoor test substance of gas；The radiation wideband light source SLD
It is connect with the input terminal of single mode optical fiber, the output end connection of the spectroanalysis instrument and multimode fibre.
Further, the photic conductive adsorbent thin film of iodine polyacetylene of mixing is coated in hollow Bragg optical fiber as follows
Fibre core inner surface on：
The first step prepares silver layer in hollow Bragg optical fiber inner walls comprising：
I, by hollow Bragg optical fiber successively in deionized water, absolute ethyl alcohol, acetone ultrasound 5min to clean interior appearance
Hollow Bragg optical fiber after cleaning is put into vacuum drying chamber by face, dry 20min under the conditions of 60 DEG C；
II, 1g SnCl accurately are weighed2·H2O, the SnCl that will be weighed2·H2O is dissolved in the dense hydrogen chloride of 5mL and 100mL go from
In the solution of sub- water composition, and appropriate tin grain is added into solution, the sensitizing solution of a concentration of 10g/L is configured to, by hollow Bragg
Optical fiber is put into sensitizing solution sensitization, then sensitization time 5min cleans hollow Bragg optical fiber with deionized water；
III, using deionized water as medium, configuration concentration be 0.3g/L palladium bichloride activating solution, hollow Bragg optical fiber is put
Enter palladium bichloride activating solution to be activated, it is 30-45 DEG C to keep temperature, and soak time is 3~8 minutes；
IV, the silver nitrate solution 10mL for preparing 3.5g/100mL, are slowly added dropwise 28% ammonium hydroxide and are just dissolved until precipitating,
38% drop of acetaldehyde 5 is added dropwise again, it is 60-80 DEG C to keep temperature, so that solution is slow transitted through at activated, sensitization by peristaltic pump
The inside of optical fibre of reason, until the silver layer of optical fiber inner wall depositing homogeneous；
Second step, preparation mix the photic conductive adsorbent thin film of iodine polyacetylene comprising：
A, by hollow Bragg optical fiber both ends rubber stopper seal, and two apertures are reserved respectively on the rubber stopper of both ends so that
Gold or platinum filament pass through electrode and electrolyte；
B, using deionized water as medium, the electrolyte with catalytic action is prepared, acetylene gas is passed through to being saturated, makes electrolysis
Liquid passes through inside of optical fibre from bottom to top；
C, using Bragg optical fiber inner wall silver layers as working electrode, gold or platinum filament are to use electrochemical workstation control to electrode
Current density processed is 1~3mAcm-2, the electrochemistry formated of polyacetylene film is carried out at room temperature；
D, current density and reaction time are controlled, until obtaining the polyacetylene film that thickness is 130nm~170nm；
E, deionized water, absolute ethyl alcohol, acetone are passed through into optical fiber to clean unreacted electrolyte, by the light after cleaning
Fibre is put into vacuum drying chamber, 2 hours dry under the conditions of 60 DEG C, is doped to polyacetylene film with iodine steam, is obtained thickness
Degree is uniform and to PM2.5Sensitive mixes the photic conductive adsorbent thin film of iodine polyacetylene.
Further, the high refractive index layer is silicon layer, and the low-index layer is silicon dioxide layer.
Beneficial effects of the present invention：
1, the present invention is based on the PM of hollow Bragg optical fiber2.5Concentration detection apparatus, hollow Bragg optical fiber and solid core photon
Crystal optical fibre is compared, the sensitivity higher of hollow Bragg optical fiber；In the air-core inner surface coating pair of hollow Bragg optical fiber
PM2.5Particle mixes iodine polyacetylene nano thin-film with photic conductive suction-operated, can give full play to the light that nano thin-film has
Irradiation enhancing PM2.5 particle absorption effect beneficials, the PM based on this formation2.5Concentration sensor shows high sensitivity, structure
The features such as simple.
2, the present invention is based on the PM of hollow Bragg optical fiber2.5Concentration detection apparatus, using electrochemical process in hollow Bragg
Fiber core inner surface, which is formed, mixes the self-assembled film of iodine polyacetylene, close by controlling the electric current of electrochemistry formated in preparation process
Degree and reaction time can accurately control the film thickness for mixing iodine polyacetylene, therefore the thickness obtained for mixing iodine polyacetylene film is uniform
Controllably, stable structure, while the film obtained is not easy to be influenced by environment temperature, pollution so that PM in air-core2.5
The detection sensitivity and accuracy higher, stability of concentration sensor are more preferable.By mixing iodine polyacetylene film to fine particle
PM2.5Controllable adsorption, hollow Bragg optical fiber wavelength modulation and refractive index high sensitivity and nano level film thickness
The combination of 130~170nm keeps transducer sensitivity height, fast response time, detection limit low.
3, the present invention is based on the PM of hollow Bragg optical fiber2.5Concentration detection apparatus, mixing iodine polyacetylene film has film layer
Thickness uniformly, high-specific surface area, it is photic negatively charged the features such as, can the firmly positively charged PM of efficient absorption2.5Particle；And
Suitable for using the larger hollow Bragg fiber laser arrays PM of core diameter (200 μm)2.5Concentration.Therefore make PM2.5Concentration sensor has
The characteristics of detection sensitivity height, fast response time.
4, the present invention is based on the PM of hollow Bragg optical fiber2.5Concentration detection apparatus is based on hollow Bragg optical fiber PM2.5It is dense
The transducing signal of degree detection belongs to wavelength modulation, can avoid light caused by supply voltage in measurement process, ambient temperature and humidity fluctuation
Signal interference；By optical fiber sensing network, it can be achieved that multi-functional, intellectualized detection.
Description of the drawings
Fig. 1 is the PM based on hollow Bragg optical fiber in embodiment2.5The structural schematic diagram of concentration detection apparatus；
Fig. 2 is the end structure illustration of hollow Bragg optical fiber；
Fig. 3 is the close-up schematic view in 1-D photon crystal layer portion in hollow Bragg optical fiber；
Fig. 4 is that hollow Bragg optical fiber 9 shows the combination of electrode 14, electrolyte input pipe 15 with rubber stopper 13, gold or platinum filament
It is intended to.
Specific implementation mode
The invention will be further described with reference to the accompanying drawings and examples.
PM of the present embodiment based on hollow Bragg optical fiber2.5Concentration detection apparatus, including superradiance wideband light source SLD 1,
Optical fiber PM2.5Concentration sensor, test gas chamber 2, PM2.5Generator 3, controlled valve 4, gas flowmeter 5,6 and of spectroanalysis instrument
The computer 7 being connect with spectroanalysis instrument.
The optical fiber PM2.5Concentration sensor is coated with by 8, air-core inner surfaces of a single mode optical fiber to be mixed iodine and gathers
9, multimode fibres 10 of hollow Bragg optical fiber and two 11 groups of optical fiber connectors of the photic conductive adsorbent thin film of acetylene 12
At the output end of single mode optical fiber is connect by optical fiber connector with the input terminal of hollow Bragg optical fiber, hollow Bragg optical fiber
Output end is connected by the input terminal of optical fiber connector and multimode fibre.
The hollow Bragg optical fiber is by a diameter of 200 μm of air-core 91, the one-dimensional light being enclosed in outside air-core
Sub- crystal layer 92, the covering 93 being enclosed in outside 1-D photon crystal layer are constituted；The 1-D photon crystal layer is by period sex-intergrade
The high refractive index layer 921 and low-index layer 922 of distribution form, and the high refractive index layer is silicon layer, and the low-index layer is
Silicon dioxide layer.The refractive index of each high refractive index layer is identical with thickness, and the refractive index and thickness of each low-index layer are also identical, should
The transmission wave band centre wavelength of hollow Bragg optical fiber is at 1.55 μm.
The optical fiber PM2.5Concentration sensor is set in test gas chamber, and air inlet is provided on the test gas chamber and is gone out
Gas port, the air inlet by controlled valve respectively with PM2.5Generator is connected with the gas flowmeter of control nitrogen flow；Institute
The both ends open end for stating hollow Bragg optical fiber is directly communicated with the test indoor test substance of gas；The radiation wideband light source SLD
It is connect with the input terminal of single mode optical fiber, the output end connection of the spectroanalysis instrument and multimode fibre.
In the present embodiment, the photic conductive adsorbent thin film of iodine polyacetylene of mixing is coated in hollow Bragg as follows
On the fibre core inner surface of optical fiber：
The first step prepares silver layer in hollow Bragg optical fiber inner walls comprising：
I, by hollow Bragg optical fiber successively in deionized water, absolute ethyl alcohol, acetone ultrasound 5min to clean interior appearance
Hollow Bragg optical fiber after cleaning is put into vacuum drying chamber by face, dry 20min under the conditions of 60 DEG C；
II, 1g SnCl accurately are weighed2·H2O, the SnCl that will be weighed2·H2O is dissolved in the dense hydrogen chloride of 5mL and 100mL go from
In the solution of sub- water composition, and appropriate tin grain is added into solution, the sensitizing solution of a concentration of 10g/L is configured to, by hollow Bragg
Optical fiber is put into sensitizing solution sensitization, then sensitization time 5min cleans hollow Bragg optical fiber with deionized water；
III, using deionized water as medium, configuration concentration be 0.3g/L palladium bichloride activating solution, hollow Bragg optical fiber is put
Enter palladium bichloride activating solution to be activated, it is 30-45 DEG C to keep temperature, and soak time is 3~8 minutes；
IV, the silver nitrate solution 10mL for preparing 3.5g/100mL, are slowly added dropwise 28% ammonium hydroxide and are just dissolved until precipitating,
38% drop of acetaldehyde 5 is added dropwise again, it is 60-80 DEG C to keep temperature, so that solution is slow transitted through at activated, sensitization by peristaltic pump
The inside of optical fibre of reason, until the silver layer of optical fiber inner wall depositing homogeneous；
Iodine polyacetylene film is mixed in second step, preparation comprising：
A, by hollow Bragg optical fiber both ends rubber stopper seal, and two apertures are reserved respectively on the rubber stopper of both ends so that
Gold or platinum filament pass through electrode and electrolyte；
B, using deionized water as medium, the electrolyte with catalytic action is prepared, acetylene gas is passed through to being saturated, makes electrolysis
Liquid passes through inside of optical fibre from bottom to top；
C, using Bragg optical fiber inner wall silver layers as working electrode, gold or platinum filament are to use electrochemical workstation control to electrode
Current density processed is 1~3mAcm-2, the electrochemistry formated of polyacetylene film is carried out at room temperature；
D, current density and reaction time are controlled, until obtaining the polyacetylene film that thickness is 130nm~170nm；
E, deionized water, absolute ethyl alcohol, acetone are passed through into optical fiber to clean unreacted electrolyte, by the light after cleaning
Fibre is put into vacuum drying chamber, 2 hours dry under the conditions of 60 DEG C, is doped to polyacetylene film with iodine steam, is obtained thickness
Degree is uniform and to PM2.5Sensitive mixes iodine polyacetylene film.
It after mixing the making of iodine polyacetylene film, removes and has been coated with the hollow Bragg optical fiber for mixing iodine polyacetylene film, use
The hollow Bragg optical fiber that optical fiber cutter Cutting Length L is 3~9cm is assemblied in and measures in gas chamber as sensitive zones.According to
Light Wave Guide Theory, when propagation constant β meets β ＜ kn1＜ kn2When, light wave can be n in refractive index1And n2Medium in normally pass
It is defeated, and encountering different media can be by different degrees of scattering.But for the light wave of specific wavelength and incidence angle, if
When dielectric layer in covering meets Bragg diffraction condition, serious scattering and interference effect will be generated, by scattering and doing
After relating to superposition, most of energy of light wave can be transmitted by being strapped in fibre core well.
Optical fiber PM in the present embodiment2.5The operation principle of concentration sensor is as follows：
The central wavelength lambda of hollow Bragg optical fibercIt can be given by：
Wherein, dhAnd dlThe respectively thickness of high refractive index material layer and low refractive index material layer, nhAnd nlRespectively height
The refractive index of refractive index material, ncFor fibre core effective refractive index.
As the PM of various concentration2.5Particle be passed through hollow Bragg fiber cores and with coated in hollow Bragg fiber cores
When mixing iodine polyacetylene film contacts of inner surface, the refractive index for mixing iodine polyacetylene film changes, and fibre core is caused effectively to reflect
Rate changes, so that the difference of two squares hair of fibre core effective refractive index and covering (being respectively height, low-index layer) refractive index
It is raw to change；Due to high refractive index material layer (silicon layer) thickness dhWith low refractive index material layer (silicon dioxide layer) thickness dlFor definite value,
Above formula hollow core Bragg fiber optic hub wavelength XscAlso it will change；It is passed through containing PM by analyte sensors2.5Nitrogen before
Rear center's wavelength XcAmount of movement Δ λ, establish PM2.5Relationship between concentration c and centre wavelength amount of movement Δ λ；Detection contains
PM2.5Nitrogen be passed through center sensor wavelength amount of movement Δ λ before and after sensor, you can obtain PM to be measured2.5Concentration.
In the present embodiment, its core diameter of the hollow Bragg optical fiber is 200 μm, and the height of 1-D photon crystal reflects
Rate material is respectively silicon and silica, and silicon and silicon dioxide layer thickness are respectively 0.125 μm and 0.34 μm, and the period number of plies is 10
Layer, cladding diameter are 610 μm, and length l is 20cm.
The photic conductive adsorbent thin film of iodine polyacetylene of mixing is high-index material, and refractive index is 1.81 or so.
The photic conductive adsorbent thin film of iodine polyacetylene of mixing is conductive, fine particle PM2.5With positive charge, so
Under the effect of SLD light sources, apparent motion of the electrons inside iodine polyacetylene film to film, therefore more PM are mixed2.5Particle
It is adsorbed onto film surface, its optical property is made to change.
It is detection PM below2.5Four specific embodiments of mass concentration.
Experimental example 1：The thickness that iodine polyacetylene film is mixed in the coating of hollow Bragg fiber core inner surfaces is 100nm, to contain
Mass concentration is 0~150 μ g/m3Fine particle PM2.5Nitrogen as object, have an effect respectively with fibre core inner wall membrane, pass
Sensor transmission spectrum resonance wavelength is with PM2.5The increase of concentration is moved to shortwave length direction.And resonance wavelength amount of movement Δ λ with
PM2.5Linear related between mass concentration c, equation of linear regression is：
Δ λ=kc+b
C is PM to be measured in formula2.5Particle concentration, Δ λ are hollow Bragg optical fiber transmission spectrum resonance wavelength amount of movements, and k is oblique
Rate, b are intercept.
Known PM is used in experiment2.5Mass concentration is 0,10 μ g/m3, 20 μ g/m3, 50 μ g/m3, 80 μ g/m3, 100 μ g/m3,
150μg/m3Nitrogen be detected, respective sensor transmission spectrum resonance wavelength amount of movement Δ λ is respectively 0,0.32,0.68,
1.76,2.4,2.88,3.60nm, equation of linear regression is：Δ λ=0.0248c+0.2120, related coefficient are：R2=
0.9693, i.e., k, b are respectively 0.0248,0.2120 in equation of linear regression.
After the nano thin-film of under test gas and hollow Bragg fiber core inner surfaces contacts, transmission spectrum resonance wavelength is flat
Equal amount of movement Δ λ is 1.28nm, can calculate PM to be measured2.5Mass concentration c=43.1 μ g/m3, 26 seconds response times, recovery
53 seconds time.
Experimental example 2：The thickness that iodine polyacetylene film is mixed in the coating of hollow Bragg fiber core inner surfaces is 150nm, and is tested
It is middle to use known PM2.5Mass concentration is 0,10 μ g/m3, 20 μ g/m3, 50 μ g/m3, 80 μ g/m3, 100 μ g/m3, 150 μ g/m3Nitrogen
Gas is detected, and sensor transmission spectrum resonance wavelength is with PM2.5The increase of concentration is moved to shortwave length direction, corresponding transmission spectrum
Resonance wavelength amount of movement Δ λ is respectively 0,0.36,0.72,1.84,2.34,2.86,3.62nm, and equation of linear regression is：Δλ
=0.0245c+0.2409, related coefficient are：R2=0.9685, i.e., k, b are respectively 0.0245 in equation of linear regression,
0.2409。
After the sensitive thin film of under test gas and hollow Bragg fiber core inner surfaces contacts, transmission spectrum resonance wavelength is flat
Equal amount of movement Δ λ is 1.12nm, can calculate PM to be measured2.5Mass concentration c=35.9 μ g/m3, 21 seconds response times, recovery
48 seconds time.
Experimental example 3：The thickness that iodine polyacetylene film is mixed in the coating of hollow Bragg fiber core inner surfaces is 170nm, and is tested
It is middle to use known PM2.5Mass concentration is 0,10 μ g/m3, 20 μ g/m3, 50 μ g/m3, 80 μ g/m3, 100 μ g/m3, 150 μ g/m3Nitrogen
Gas is detected, and sensor transmission spectrum resonance wavelength is with PM2.5The increase of concentration is moved to shortwave length direction, corresponding transmission spectrum
Resonance wavelength amount of movement Δ λ is respectively 0,0.34,0.66,1.84,2.36,2.82,3.56nm, and equation of linear regression is：Δλ
=0.0243c+0.2293, related coefficient are：R2=0.9645, i.e., k, b are respectively 0.02434 in equation of linear regression,
0.2293。
After the nano thin-film of under test gas and hollow Bragg fiber core inner surfaces contacts, transmission spectrum resonance wavelength is flat
Equal amount of movement Δ λ is 1.40nm, can calculate PM to be measured2.5Mass concentration c=48.2 μ g/m3, 28 seconds response times, recovery
55 seconds time.
Experimental example 4：The thickness that iodine polyacetylene film is mixed in the coating of hollow Bragg fiber core inner surfaces is 200nm, and is tested
It is middle to use known PM2.5Mass concentration is 0,10 μ g/m3, 20 μ g/m3, 50 μ g/m3, 80 μ g/m3, 100 μ g/m3, 150 μ g/m3Nitrogen
Gas is detected, and sensor transmission spectrum resonance wavelength is with PM2.5The increase of concentration is moved to shortwave length direction, corresponding transmission spectrum
Resonance wavelength amount of movement Δ λ is respectively 0,0.26,0.58,1.74,2.28,2.80,3.50nm, and equation of linear regression is：Δλ
=0.0243c+0.1700, related coefficient are：R2=0.9679, i.e., k, b are respectively 0.0243 in equation of linear regression,
0.1700。
After the nano thin-film of under test gas and hollow Bragg fiber core inner surfaces contacts, transmission spectrum resonance wavelength is flat
Equal amount of movement Δ λ is 1.96nm, can calculate PM to be measured2.5Mass concentration c=73.7 μ g/m3, 31 seconds response times, recovery
72 seconds time.
Claims (3)
1. a kind of PM based on hollow Bragg optical fiber2.5Concentration detection apparatus, it is characterised in that：Including superradiance wideband light source
SLD, optical fiber PM2.5Concentration sensor, test gas chamber, PM2.5Generator, controlled valve, gas flowmeter, spectroanalysis instrument and with
The computer of spectroanalysis instrument connection；
The optical fiber PM2.5Concentration sensor is coated with by a single mode optical fiber, an air-core inner surface and is mixed iodine polyacetylene light
The hollow Bragg optical fiber, a multimode fibre and two optical fiber connector compositions of conductive adsorbent thin film are caused, single mode optical fiber
Output end is connect by optical fiber connector with the input terminal of hollow Bragg optical fiber, and the output end of hollow Bragg optical fiber passes through optical fiber
The input terminal of connector and multimode fibre connects；
The hollow Bragg optical fiber is by a diameter of 200 μm of air-core, the 1-D photon crystal being enclosed in outside air-core
Layer, the covering being enclosed in outside 1-D photon crystal layer are constituted；The 1-D photon crystal layer is rolled over by the height of periodical cross-distribution
Penetrate rate layer and low-index layer composition, the refractive index of each high refractive index layer is identical with thickness, the refractive index of each low-index layer and
Thickness is also identical, and the transmission wave band centre wavelength of hollow Bragg optical fiber is at 1.55 μm；
The optical fiber PM2.5Concentration sensor is set in test gas chamber, and air inlet and outlet are provided on the test gas chamber
Mouthful, the air inlet by controlled valve respectively with PM2.5Generator is connected with the gas flowmeter of control nitrogen flow；It is described
The both ends open end of hollow Bragg optical fiber is directly communicated with the test indoor test substance of gas；The radiation wideband light source SLD with
The input terminal of single mode optical fiber connects, and the output end of the spectroanalysis instrument and multimode fibre connects.
2. the PM according to claim 1 based on hollow Bragg optical fiber2.5Concentration detection apparatus, it is characterised in that：It is described
The photic conductive adsorbent thin film of iodine polyacetylene is mixed to be coated on the fibre core inner surface of hollow Bragg optical fiber as follows：
The first step prepares silver layer in hollow Bragg optical fiber inner walls comprising：
I, by hollow Bragg optical fiber, ultrasound 5min, will to clean surfaces externally and internally in deionized water, absolute ethyl alcohol, acetone successively
Hollow Bragg optical fiber after cleaning is put into vacuum drying chamber, dry 20min under the conditions of 60 DEG C；
II, accurately 1g stannous chlorides (SnCl is weighed2·H2O), the SnCl that will be weighed2·H2O is dissolved in the dense hydrogen chloride of 5mL and 100mL
In the solution of deionized water composition, and appropriate tin grain is added into solution, the sensitizing solution of a concentration of 10g/L is configured to, by hollow
Bragg optical fiber is put into sensitizing solution sensitization, then sensitization time 5min cleans hollow Bragg optical fiber with deionized water；
III, using deionized water as medium, configuration concentration be 0.3g/L palladium bichloride activating solution, hollow Bragg optical fiber is put into chlorine
Change palladium activating solution to be activated, it is 30-45 DEG C to keep temperature, and soak time is 3~8 minutes；
28% ammonium hydroxide is slowly added dropwise until precipitation just dissolves, then drips in IV, the silver nitrate solution 10mL for preparing 3.5g/100mL
38% acetaldehyde 5 is added to drip, it is 60-80 DEG C to keep temperature, so that solution is slow transitted through by peristaltic pump activated, sensitized treatment
Inside of optical fibre, until the silver layer of optical fiber inner wall depositing homogeneous；
Iodine polyacetylene film is mixed in second step, preparation comprising：
A, by hollow Bragg optical fiber both ends rubber stopper seal, and two apertures are reserved respectively on the rubber stopper of both ends so that Jin Huo
Platinum filament passes through electrode and electrolyte；
B, using deionized water as medium, the electrolyte with catalytic action is prepared, acetylene gas is passed through to being saturated, makes electrolyte certainly
Pass through inside of optical fibre on down；
C, using Bragg optical fiber inner wall silver layers as working electrode, gold or platinum filament are to use electrochemical operation stand control electricity to electrode
Current density is 1~3mAcm-2, the electrochemistry formated of polyacetylene film is carried out at room temperature；
D, current density and reaction time are controlled, until obtaining the polyacetylene film that thickness is 130nm~170nm；
E, it is passed through deionized water, absolute ethyl alcohol, acetone into optical fiber to clean unreacted electrolyte, the optical fiber after cleaning is put
Enter in vacuum drying chamber, it is 2 hours dry under the conditions of 60 DEG C, polyacetylene film is doped with iodine steam, it is equal to obtain thickness
It is even and to PM2.5Sensitive mixes iodine polyacetylene film.
3. the PM according to claim 1 based on hollow Bragg optical fiber2.5Concentration detection apparatus, it is characterised in that：It is described
High refractive index layer is silicon layer, and the low-index layer is silicon dioxide layer.
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