CN109900641A - A kind of poly- hexamethyl biguanides film package microsphere resonator CO2Sensor and manufacture craft - Google Patents
A kind of poly- hexamethyl biguanides film package microsphere resonator CO2Sensor and manufacture craft Download PDFInfo
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Abstract
A kind of poly- hexamethyl biguanides film package microsphere resonator CO2Sensor and manufacture craft, 1) micro-nano fiber coupler (1) and plated film microsphere resonator (2) on concave glass plate will be fixed on to fix on three-D displacement platform respectively；2) micro-nano fiber both ends are separately connected wideband light source and spectrometer, observation spectrum and the position for adjusting microsphere resonator (2), micro-nano fiber is fixed on concave poly (methyl methacrylate) plate with ultraviolet glue, region adjustment is girdled the waist in the central location of concave poly (methyl methacrylate) plate in position by controlling micro-nano fiber, and poly- hexamethyl biguanides solution drop is formed microsphere resonator (2) in fiber optic microsphere；3) then structure made of step 2 is fixed on by the cuboid of 3D printing poly (methyl methacrylate) plate gas chamber with cover, lid seals gas chamber；4) two air cavity packages gas concentrations that air inlet pipe and escape pipe are separately connected gas chamber are tested.The shortcomings that overcoming optical microcavity that can not directly be detected to density of carbon dioxide gas, structure is simple, it is highly sensitive and can long-term work in room temperature environment.
Description
Technical field
The invention belongs to fiber optic sensor technology fields, and in particular to a kind of poly- hexamethyl biguanides film package microballoon resonance
Chamber CO2Sensor and manufacture craft.
Background technique
Since the industrial revolution, the greenhouse gases that the mankind discharge into atmosphere increase sharply year by year, and greenhouse effects cause entirely
Ball climate warming, sea level rise, adverse weather, Marine Storm Genesis increase and desertification area increase etc. a series of serious problems,
Cause the concern of whole world various countries.
Carbon dioxide is with 77% discharge than occupying main greenhouse gases.Carbon dioxide greenhouse effect and global climate become
The warm common concern for having caused countries in the world currently promotes and works out international climate change pact, reduces carbon dioxide
Discharge have become trend of the times.China is in the critical period of industrialization, urbanization process, economic development bring energy
Source consumption and resulting carbon emission problem are by domestic and international common concern.
2014, China had become global the first big country of carbon emission.Can China avoid repeating the development of developed country
Mode goes on stabilization, low-carbon, sustainable development road, is one of the critical issue of world's reply climate change.CCS technology
(Carbon Capture and Storage) is by carbon dioxide (CO2) capture, the technology sealed up for safekeeping.CCS technology, which refers to, to be passed through
Carbon capture technology comes out industry and related energy industry carbon dioxide separation produced, will then by Carbon stock means
It conveys and seals up for safekeeping to the place of the inferior isolation atmosphere in seabed or ground.Currently, CCS technology is still in development phase.Wherein, two
During carbonoxide geological storage and the controlling of injecting quantity, implementing quickly and effectively detection to density of carbon dioxide gas is to prevent
The technological difficulties of carbon dioxide leakage.
The advantages that optical sensing technology has detection quickly, high sensitivity, electromagnetism interference monitors field in gas concentration
With extensive.According to sensor mechanism difference, optical gas sensing can be divided into based on absorption spectrum and refractometry two types.
Based on the optical sensor of absorption spectrum method since its spectral absorption peak is not influenced vulnerable to the other factors outside degasification bulk concentration,
By extensive commercial.
But spectral absorption method is higher to light source and request detector, especially infrared in gas absorption intensity is higher
Wave band, associated op-tics price is costly.For example, carbon dioxide gas absorbs by force optical wavelength respectively in 4.2 μm and 2.0 μm
Near, and it is relatively weak in communication band (1.567 μm) absorption peak strength, it is lower using spectral absorption method detection limit.Refraction
Rate mensuration realizes the inspection to gas concentration using variations in refractive index caused by detection gas and gas sensitive interaction
It surveys, and operation wavelength is unrestricted, it is compatible with communication device.
In recent years, with the continuous maturation of micro-processing technology, it is based on optics Whispering-gallery-mode (Whispering Gallery
Mode, WGM) microcavity optical sensing technology as a kind of high sensitivity, the novel optical sensor mechanism of low detection limits is wide
General research and the detection for being applied to high-sensitivity biological chemistry.Although optical microcavity refractive index sensitivity with higher,
Still can not detection gas concentration directly change caused variations in refractive index, and gas-selectively detection can not be carried out.It will
Carbon dioxide gas sensor material is combined with optics Whispering-gallery-mode microcavity, utilizes the highly sensitive refractive index of Whispering-gallery-mode microcavity
Sensing characteristics have great significance to the density of carbon dioxide gas monitoring for realizing highly sensitive and low detection limits.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the object of the present invention is to provide a kind of poly- hexamethyl biguanides films to wrap up
Microsphere resonator CO2Sensor and manufacture craft overcome optical microcavity that can not directly be detected to density of carbon dioxide gas
The shortcomings that, have structure it is simple, it is highly sensitive and can long-term work in room temperature environment.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of poly- hexamethyl biguanides film package microsphere resonator CO2Sensor, including concave poly (methyl methacrylate) plate, micro-nano fiber are logical
It crosses UV glue and is fixed on concave poly (methyl methacrylate) plate, micro-nano fiber is girdled the waist, and region is centrally located, and microsphere resonator surface plates one layer
Poly- hexamethyl biguanides coating is fixed on concave poly (methyl methacrylate) plate；Microsphere resonator contacts micro-nano fiber place with a tight waist.
A kind of poly- hexamethyl biguanides film package microsphere resonator CO2The manufacture craft of sensor, comprising the following steps:
1) micro-nano fiber and microsphere resonator on concave glass plate will be fixed on to fix on three-D displacement platform respectively；
2) micro-nano fiber both ends are separately connected wideband light source and spectrometer, observe spectrum and adjust the position of microsphere resonator,
Make to contact micro-nano fiber place with a tight waist, about 2 μm of the beam waist diameter of the micro-nano fiber, micro-nano fiber is fixed on ultraviolet glue recessed
On type poly (methyl methacrylate) plate, the position place of being girdled the waist by controlling micro-nano fiber is adjusted in the central position of concave poly (methyl methacrylate) plate
It sets, poly- hexamethyl biguanides solution drop is formed into microsphere resonator in fiber optic microsphere；
3) then structure made of step 2 is fixed on by the cuboid of 3D printing poly (methyl methacrylate) plate gas chamber with cover, lid
Gas chamber is sealed；
4) air inlet pipe and escape pipe are separately connected to two stomatas of gas chamber, it is micro- that the optical fiber based on poly- hexamethyl biguanides film is made
Cavity resonance CO2Sensor.
The micro-nano fiber draws cone to be made by standard single-mode fiber through flame, made of single mode optical fiber discharges through heat sealing machine
Microsphere resonator and poly- hexamethyl biguanides air-sensitive film.
The microsphere resonator is that the commercial single mode optical fiber (SM-28) for cutting flat with end face obtains after heat sealing machine multiple discharge
To about 170 μm of microballoon of diameter.
The poly- hexamethyl biguanides solution prepares poly- hexamethyl biguanides air-sensitive film via rotary coating, and poly- hexamethyl is double
Guanidine solution is configured to after supersonic cleaning machine is heated to 40 DEG C of ultrasound 30min by poly- hexamethyl biguanides powder and deionized water
30% solution, the microballoon for coating poly- hexamethyl biguanides are to drip poly- hexamethyl biguanides solution in the light for being fixed on desk-top sol evenning machine
On fine microballoon, the thickness of film is controlled by the revolving speed of desk-top spin coating.
The beneficial effects of the present invention are:
The present invention is by highly sensitive echo wall mode optical micro-cavity sensing arrangement and poly- hexamethyl biguanides carbon dioxide gas sensor material
Material combines.Surface is coupled light into coated with poly- hexamethyl biguanides by the micro-nano fiber being fixed on concave poly (methyl methacrylate) plate
In microsphere resonator.Wherein, the beam waist diameter of micro-nano fiber is about 2 μm, is efficiently coupled the light into microsphere resonator.Poly- six
Effectively with carbon dioxide reversible reaction can occur for methyl biguanides organic matter at normal temperatures and pressures.Poly- hexamethyl biguanides and dioxy
Change carbon reaction and change the refractive index of microsphere resonator surface film, and then change the stationary field being strapped in microballoon, shows
For the drift at resonant cavity spectral resonance peak.Therefore, fiber optic microsphere resonator sensor based on poly- hexamethyl biguanides film can be with
Effective detection density of carbon dioxide gas.The sensor can substitute traditional middle infrared spectrum absorption-type gas sensor narrow
Density of carbon dioxide gas detection is carried out in small space environment.
Detailed description of the invention
Fig. 1 is 2 μm of micro-nano fibers production schematic diagram of the invention.
Fig. 2 is the micrograph of microballoon Whispering-gallery-mode resonance structure of the invention.
Fig. 3 is the structural schematic diagram of the embodiment of the present invention 1.
Fig. 4 is spectrogram of the embodiment of the present invention 1 in pure nitrogen gas environment.
Fig. 5 is that the embodiment of the present invention 1 responds in 1550nm wave band response diagram the gas concentration lwevel test of 0-600ppm.
Fig. 6 is the experimental result data fitted figure of the embodiment of the present invention 1.
Specific embodiment
With reference to embodiments and attached drawing is further discussed below the present invention.
A kind of fiber optic microsphere resonant cavity carbon dioxide gas sensor based on poly- hexamethyl biguanides film of the present embodiment
Including micro-nano fiber 1, microsphere resonator 2 and the connection of concave poly (methyl methacrylate) plate 3 are constituted.
Embodiment 1
As shown in Figure 1, micro-nano fiber 1 is made of that standard single-mode fiber is drawn cone motorized stage system by flame in the present embodiment.
Wherein, cone motorized stage system is drawn to be made of two one dimension displacement platforms and mating lifting platform, wherein the edge respectively of electricity driving displacement platform 1,2
One axis is two-way to be placed in parallel, and is stretched for controlling the left and right of optical fiber, installed on electricity driving displacement platform respectively a Two-dimensional Position moving stage and
Fibre clip, for the left and right for fixing and controlling optical fiber and fine tuning up and down.The fixed flame gun of electricity driving displacement platform 3 and adjustable fire
The upper and lower and left-right position of flame.Flame gun uses butane fuel, and temperature is up to 1300 DEG C or so (being enough fused optic fiber).It is electronic
Displacement platform 1,2 controls the speed of service and range ability by computer.Optical fiber is placed in the position of flame internal flame, and electricity driving displacement platform
1,2 speed of service and range ability are controlled as 1 mm/s and 12 mm, and optical taper area beam waist diameter can be obtained and be about 2
μm micro-nano fiber 1.It then, will be in the center modulation micro-nano fiber of concave poly (methyl methacrylate) plate 3 by control three-D displacement platform
Position is entreated, cone area is hanging and probably determines regional location with a tight waist.Then micro-nano fiber both ends are fixed with ultraviolet glue.Microballoon resonance
Chamber 2 is to cut flat with commercial 1550 nm fiber end faces, then using heat sealing machine through 5 bit of strength of discharge, 1500 ms of discharge time,
After 4 continuous discharge, about 170 μm of diameter of microballoon is obtained.Poly- hexamethyl biguanides solution be by poly- hexamethyl biguanides powder with go
Ionized water is configured to 30% poly- hexamethyl biguanides solution after supersonic cleaning machine is heated to 40 DEG C of 30 min of ultrasound.Microballoon is pressed from both sides
Among triangular pyramid block, triangular pyramid block is fixed in desk-top sol evenning machine with glue, the revolving speed control of sol evenning machine is 1500 rad/s,
Time is 30s, obtains microsphere resonator 2.
The structure of sensor as shown in figure 3, will be fixed on micro-nano fiber 1 and microballoon on concave glass plate in the present embodiment
Resonant cavity 2 is fixed on three-D displacement platform respectively, micro-nano fiber both ends is separately connected wideband light source and spectrometer, observation spectrum is simultaneously
The position for adjusting microsphere resonator 2, is finally fixed with ultraviolet glue, Fig. 2 provides the micro-structure diagram of the sensor.The light of sensor
Spectrogram is as shown in Figure 4.Then sensor is fixed on by the cuboid of 3D printing poly (methyl methacrylate) plate gas chamber with cover, lid will
Gas chamber seals, and air inlet pipe and escape pipe are finally separately connected to two stomatas of gas chamber.
Example 2
In the present embodiment, the beam waist diameter of micro-nano fiber 1 is 2 μm, builds the concrete operations and 1 phase of embodiment of microballoon resonance
Together, microsphere resonator 2 is replaced by diameter by 125 μm of 1550nm wave band general commercial single mode optical fiber.
Experimental conditions are as follows:
Laboratory apparatus: fiber Bragg grating (FBG) demodulator, model SM-125 are produced by MICRON OPTICS company；5 sccm and 2000
The mass flow controller of sccm, model OLCSA05292, is produced by Beijing Qixing Huachuang Electronics Co., Ltd；It is desk-top even
Glue machine, model KW-4A, the production of You Zhongpu Buddhist nun's intelligent technology limited；Digital ultrasound cleaning machine, model TH-100B, by
The production of Jinan Pu Na Instrument and Equipment Company.
Chemical example: poly- hexamethyl biguanides (PHMB), Suzhou indigo plant space chemical industry.
1, density of carbon dioxide gas measurement experiment
The carbon dioxide sensor that the present invention makes is placed in constant temperature gas chamber, constant temperature is 25 DEG C.It is determined in air inlet pipe
The carbon dioxide gas of concentration is to modulate control ratio by mass flow controller by carbon dioxide and nitrogen.Carbon dioxide and nitrogen
It each leads into the mass flow controller of 5 sccm and 2000 sccm.The air inlet carbon dioxide of computer regulated mass flow controller
Concentration.The gas concentration lwevel section experimental results of 0-600 ppm are as shown in Figure 5.Fig. 6 provides the sensitivity of the sensing about
0.00324 pm/ppm。
Working principle of the present invention is as follows:
Optical Microsphere resonant cavity is a kind of based on Whispering-gallery-mode principle, and light is bound by the photon that resonance is carried out in short space
Learn device.The spectral characteristic of Optical Microsphere resonant cavity shows as a series of resonance peaks of equal frequency intervals, resonance peak wavelength with it is humorous
Vibration intracavity modal effective refractive index and resonant cavity size are related.When the air-sensitive thin polymer film adhered on microsphere resonator,
Chemical reaction will be generated with carbon dioxide gas molecule in carbon dioxide gas environment, wherein the refractive index of film or thickness will
It can change, further result in the wave length shift of resonance peak.Therefore, pass through the available titanium dioxide of drift of measurement resonance peak
Carbon gas concentration change information.
Claims (5)
1. a kind of poly- hexamethyl biguanides film wraps up microsphere resonator CO2Sensor, including concave poly (methyl methacrylate) plate (3), feature
It is, micro-nano fiber (1) is fixed on concave poly (methyl methacrylate) plate (3) by UV glue, and micro-nano fiber (1) is girdled the waist the centrally located position in region
It sets, microsphere resonator (2) surface is plated a strata hexamethyl biguanides coating (4) and is fixed on concave poly (methyl methacrylate) plate (3)；Microballoon is humorous
Chamber (2) contact micro-nano fiber (1) of shaking place with a tight waist.
2. a kind of poly- hexamethyl biguanides film of base wraps up microsphere resonator CO2The manufacture craft of sensor, which is characterized in that including
Following steps:
1) micro-nano fiber (1) and microsphere resonator (2) on concave glass plate will be fixed on to fix on three-D displacement platform respectively；
2) micro-nano fiber both ends are separately connected wideband light source and spectrometer, observe spectrum and adjust the position of microsphere resonator (2)
It sets, makes to contact micro-nano fiber (1) place with a tight waist, about 2 μm of the beam waist diameter of the micro-nano fiber, micro-nano fiber ultraviolet glue be consolidated
It is scheduled on concave poly (methyl methacrylate) plate, the position place of being girdled the waist by controlling micro-nano fiber adjusts in concave poly (methyl methacrylate) plate
Position is entreated, poly- hexamethyl biguanides solution drop is formed into microsphere resonator (2) in fiber optic microsphere；
3) then structure made of step 2 is fixed on by the cuboid of 3D printing poly (methyl methacrylate) plate gas chamber with cover, lid
Gas chamber is sealed；
4) air inlet pipe and escape pipe are separately connected to two stomatas of gas chamber, it is micro- that the optical fiber based on poly- hexamethyl biguanides film is made
Cavity resonance CO2Sensor.
3. the poly- hexamethyl biguanides film of a kind of base according to claim 2 wraps up microsphere resonator CO2The production work of sensor
Skill, which is characterized in that the micro-nano fiber draws cone to be made by standard single-mode fiber through flame, and single mode optical fiber discharges through heat sealing machine
Manufactured microsphere resonator and poly- hexamethyl biguanides air-sensitive film.
4. the poly- hexamethyl biguanides film of a kind of base according to claim 2 wraps up microsphere resonator CO2The production work of sensor
Skill, which is characterized in that the microsphere resonator is that the commercial single mode optical fiber (SM-28) for cutting flat with end face is repeatedly put through heat sealing machine
About 170 μm of diameter of microballoon is obtained after electricity.
5. the poly- hexamethyl biguanides film of a kind of base according to claim 2 wraps up microsphere resonator CO2The production work of sensor
Skill, which is characterized in that the poly- hexamethyl biguanides solution prepares poly- hexamethyl biguanides air-sensitive film via rotary coating, and poly- six
Methyl biguanides solution is by poly- hexamethyl biguanides powder and deionized water, after supersonic cleaning machine is heated to 40 DEG C of ultrasound 30min
It is configured to 30% solution, the microballoon for coating poly- hexamethyl biguanides is that poly- hexamethyl biguanides solution drop is being fixed on desk-top spin coating
On the fiber optic microsphere of machine, the thickness of film is controlled by the revolving speed of desk-top spin coating.
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| CN112113923A (en) * | 2020-09-24 | 2020-12-22 | 中山大学 | Micro-bubble cavity coupling CO based on whispering gallery mode2Sensor and manufacturing method |
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| CN112683793A (en) * | 2020-12-09 | 2021-04-20 | 哈尔滨工程大学 | Sensor for detecting concentration of liquid drops based on double-microsphere coupling mode splitting |
| CN113398347A (en) * | 2021-07-26 | 2021-09-17 | 山东大学 | Guiding type artificial oropharynx channel sputum suction device and working method |
| CN117470288A (en) * | 2023-11-02 | 2024-01-30 | 广东海洋大学 | Batch manufacturing method of membrane type Fabry-Perot interference and FBG multiplexing optical fiber sensor |
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Application publication date: 20190618 |