CN105203462A - Oxygen monitoring device and monitoring method thereof - Google Patents
Oxygen monitoring device and monitoring method thereof Download PDFInfo
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- CN105203462A CN105203462A CN201510616546.4A CN201510616546A CN105203462A CN 105203462 A CN105203462 A CN 105203462A CN 201510616546 A CN201510616546 A CN 201510616546A CN 105203462 A CN105203462 A CN 105203462A
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Abstract
The invention provides an oxygen monitoring device and a monitoring method thereof. A laser generator in the device divides a generated laser into two paths through a 2*2 coupler, wherein one path of the laser is used as signal light to be sequentially input to the 2*2 coupler, a micro-nanofiber composite structure and a signal light detector, and the other path of the laser is used as reference light to be input to a reference light detector used for detecting the intensity of the reference light. The signal light detector is electrically connected with an amplifier, a differential, an AD converter, a phase-locked modulator and a microcomputer in sequence. According to the oxygen monitoring device and the monitoring method thereof, the transmission characteristic of surface evanescent waves of the device is influenced through change of the physicochemical property of a sensitive material on the surface of the micro-nanofiber composite structure, so that oxygen sensing is achieved. The precision is high, response is fast, the special requirement for oxygen monitoring can be met, and real-time online measurement which is easy to integrate and expand, high in sensitivity and accurate in distribution can be achieved.
Description
Technical field
The present invention relates to a kind of oxygen monitoring device and monitoring method thereof.
Background technology
The gases such as detection oxygen have application widely in Industry Control, medical science, environmental monitoring and the field such as protection and biological chemistry, therefore develop quick, sensitive, efficient oxygen detection technique and method and have very important significance.At present, the oxygen measurement method applied mainly comprises titrimetry, amperometry and optical method etc.
Titrimetry is proposed for measuring oxygen in water concentration first by Winkler.The method is always by the standard method lasting for years measured as dissolved oxygen concentration.But this method operating difficulties, waste time and energy, disturbing factor is many, dependence experience, and not easily realizes on-line real time monitoring, is mainly used in the mensuration of oxygen in aqueous phase.
Amperometry is proposed for DO determination first by Heyrovsky.The method mainly determines the relation between dissolved oxygen concentration and strength of current, through repeatedly improving, makes the method constantly perfect, but the electrode volume of the method is large, and corresponding equipment miniaturization is very difficult.It is pointed out that two kinds of above-mentioned methods and other method grown up on its basis are in use subject to the interference of the factor such as external electrical field, magnetic field.Also there is potential safety hazard when using in inflammable, explosive environments simultaneously.By contrast, optical method has the advantages such as accuracy of detection is high, easy to operate, antijamming capability is strong.
In optical method, microsphere sensor, all phase are highly sensitive with it, good selective is applied in the selective enumeration method of oxygen, but two kinds of sensors are difficult to device, are easy to pollute system to be measured and reuse the shortcomings such as rate variance and limit it and further develop.
Summary of the invention
For overcoming being easily disturbed in prior art in oxygen monitoring, being difficult to device, repeat usage, being easy to pollute the deficiencies such as system to be measured, the invention provides a kind of oxygen monitoring device, another object of the present invention is to provide a kind of oxygen monitoring method, can the concentration of accurate measurements oxygen.
Oxygen monitoring device of the present invention, be characterized in, described monitoring device comprises generating device of laser, 2 × 2 coupling mechanisms 3, micro-nano fiber composite structure sensing unit 4, flashlight detector 5, reference light detector 11, amplifier 6, difference engine 7, AD converter 8, phase locking modulator 9, microcomputer 10, and wherein generating device of laser contains narrow linewidth laser 1, fibre optic isolater 2; The output terminal of described narrow linewidth laser 1 is by after Fiber connection to fibre optic isolater 2, connect the first port of 2 × 2 coupling mechanisms 3,2 × 2 coupling mechanisms 3 the 3rd port is connected with micro-nano fiber composite structure sensing unit 4 by optical fiber, 4th port of 2 × 2 coupling mechanisms 3 is connected with reference light detector 11 by optical fiber, and flashlight detector 5 is connected with micro-nano fiber composite structure sensing unit 4 by optical fiber; Flashlight detector 5 is connected with amplifier 6, difference engine 7, AD converter 8, phase locking modulator 9, microcomputer 10 successively.
Described narrow linewidth laser 1 is electrically connected with phase locking modulator 9, exports electric signal synchronous with the input electrical signal of generating device of laser for phase locking modulator 9.
Described micro-nano fiber composite structure sensing unit 4 is by micro-nano fiber and collosol and gel chlorination tris (bipyridine) ruthenium Ru (dpp)
3cl
2potpourri forms.
The diameter of described micro-nano fiber composite structure sensing unit 4 is 1 ~ 4 μm, micro-nano fiber surface collosol and gel chlorination tris (bipyridine) ruthenium Ru (dpp)
3cl
2the thickness of potpourri is 150nm.
Described generating device of laser is by 2 × 2 coupling mechanisms 3, occurred laser is divided into two-way, the road that separates inputs to micro-nano fiber composite structure sensing unit 4, flashlight detector 5 successively as flashlight, and an other road is as the reference light detector 11 inputed to reference to light for detecting reference light intensity.
Obtain amplifier 6, difference engine 7, AD converter 8 and phase locking modulator 9 in the present invention to be integrated in monitoring platform.
A monitoring method for oxygen monitoring device, is characterized in that, comprises the following steps successively:
A). be that the general single mode fiber SMF-28 of 125 microns utilizes scanning melting to draw cone farad to make the micro-nano fiber that diameter is 1 ~ 4 μm by diameter;
B). by chlorination tris (bipyridine) ruthenium Ru (dpp)
3cl
2be dissolved in absolute ethyl alcohol according to the ratio of volume ratio 1:1 and obtain mixed solution, then mixed solution is mixed according to the ratio of volume ratio 1:50 with the sol gel solution of preparation, abundant stirring and dissolving;
C). by the micro-nano fiber drawn, utilize czochralski method plated film, thicknesses of layers 150nm, and encapsulate, obtain oxygen micro-nano fiber composite structure sensing unit;
D). the laser occurred by generating device of laser connects micro-nano fiber composite structure as flashlight;
E). micro-nano fiber composite structure connects the flashlight detector being used for detection signal light intensity;
F). generating device of laser produces laser, the laser produced transfers to flashlight detector by micro-nano fiber composite structure, divided by reference light detector testing result, flashlight detector testing result show that the micro-nano fiber composite structure rete physicochemical property caused by oxygen concentration difference change and the light energy output variable quantity of generation;
G). utilize time-domain finite difference to obtain the concentration of oxygen according to the variable quantity of light energy output.
The invention has the beneficial effects as follows, device of the present invention utilizes oxygen sensitive material chlorination tris (bipyridine) ruthenium Ru (dpp) based on the large evanescent wave characteristic of micro-nano fiber
3cl
2and loading material collosol and gel carries out sensing, by the change of the physicochemical property of potpourri, the transport property affecting micro-nano fiber surface evanescent wave realizes sensing.Monitoring device of the present invention and monitoring method overcome and are easily disturbed, are difficult to device, reuse the shortcomings such as rate variance, can realize highly sensitive, the fast-response of oxygen, accurate distribution and On-line sampling system.
Accompanying drawing explanation
fig. 1for structural representation of the present invention
figure;
fig. 2for the signal of micro-nano fiber composite structure
figure;
fig. 3for
fig. 2in I-I partial enlargement
figure;
fig. 4for automation mechanized operation program of the present invention;
in figure, 1. narrow linewidth laser 2. fibre optic isolater 3.2 × 2 coupling mechanism 4. micro-nano fiber composite structure sensing unit 5. flashlight detector 11. reference light detector 6. amplifier 7. difference engine 8.AD converter 9. phase locking modulator 10. microcomputer 11. micro-nano fiber 12. sol-gel films 13. that adulterates adulterates collosol and gel particle.
Embodiment
Below in conjunction with
accompanying drawingthe present invention is described further
Embodiment 1
fig. 1for structural representation of the present invention
figure,
fig. 1in, oxygen sensor device of the present invention comprises generating device of laser, 2 × 2 coupling mechanisms 3, micro-nano fiber composite structure sensing unit 4, flashlight detector 5, reference light detector 11, amplifier 6, difference engine 7, AD converter 8, phase locking modulator 9, microcomputer 10, and wherein generating device of laser contains narrow linewidth laser 1, fibre optic isolater 2.After the output terminal of described narrow linewidth laser 1 is connected with fibre optic isolater 2 by optical fiber, connect the first port of 2 × 2 coupling mechanisms 3, the 4th port of 2 × 2 coupling mechanisms 3 is connected with reference light detector 11 by optical fiber; 3rd port of 2 × 2 described coupling mechanisms 3 by optical fiber and micro-nano fiber composite structure sensing unit 4, connection signal photo-detector 5; Described flashlight detector 5 is connected with amplifier 6, difference engine 7, AD converter 8, phase locking modulator 9, microcomputer 10 successively.
Described narrow linewidth laser 1 is electrically connected with phase locking modulator 9, synchronous with the input signal of narrow linewidth laser 1 to keep phase locking modulator 9 to output signal;
Described micro-nano fiber composite structure sensing unit 4 is made up of micro-nano fiber 11 and doping sol-gel films 12, mainly through blending method and czochralski method, potpourri is coated on micro-nano fiber 11 surface to form composite structure;
In the present embodiment, micro-nano fiber composite structure sensing unit 4 diameter is 2 μm. doping sol-gel films 12 thickness is 150nm.
A kind of oxygen sensor device and method for sensing, comprise the following steps successively:
A). general single mode fiber SMF-28 is placed on the micro-nano fiber built and draws on platform, utilize heating source that optical fiber is heated to 1200 DEG C, then the program of establishment is utilized to control drawing platform, general single mode fiber is drawn into gradually the comparatively thin and micro-nano fiber 11 preferably of diameter uniformity based on scanning method, diameter is 2 μm, and tentatively encapsulates.
B). by chlorination tris (bipyridine) ruthenium Ru (dpp)
3cl
2be dissolved in absolute ethyl alcohol according to the ratio of mass ratio 1:1, abundant stirring and dissolving, then incorporate in the sol gel solution prepared, maintain the temperature at 80 DEG C, use magnetic stirrer 1h, make Ru (dpp)
3cl
2fully be dissolved in the middle of solution, form doping Ru (dpp)
3cl
2solution.The polymer sol-gel that polycondensation reaction produces doping is constantly there is between molecule;
C). the micro-nano fiber tentatively encapsulated is placed on lift coating machine support, with pull rate 350mm/min, lift plated film is carried out to micro-nano fiber surface, the thickness of the transmittance curve of test sample to lift plated film is utilized to calculate, the thickness that can obtain the rete on micro-nano fiber surface is 150nm, put into sealed cabinet and carry out ammonia treatment 24h, then micro-nano fiber composite structure sensing unit is packaged into micro-nano fiber composite structure;
D). micro-nano fiber composite structure sensing unit 4 is connected in light path;
E). the laser sent by generating device of laser is as flashlight, be connected to 2 × 2 coupling mechanisms 3, the light sent by generating device of laser is divided into two-way, and a road is connected to micro-nano fiber composite structure sensing unit 4 as flashlight, and another road is connected to reference light detector 11 as with reference to light;
F). the flashlight that generating device of laser sends is by micro-nano fiber composite structure sensing unit 4, be connected to the flashlight detector 5 for detection signal light intensity, the energy variation that flashlight detector 5 detects the evanscent field shake caused by oxygen concentration difference and causes; By the reference light detector 11 that 2 × 2 coupling mechanisms 3 connect, while flashlight detector 5 detection signal light, the Strength Changes of the laser that reference light detector 11 detection laser generating means sends, reference light detector 11 testing result divided by flashlight detector 5 result for eliminating the caused power jitter of generating device of laser itself, avoid external environment on the impact of generating device of laser, finally obtain micro-nano fiber compound structure film optical power change caused under different oxygen concentration;
G). the different added losses obtained under utilizing time-domain finite difference (3D-FDTD) to calculate different oxygen concentration, finally obtain the form of a similar database in the present embodiment, the corresponding added losses value of each oxygen concentration, when flashlight detector 5 detects flashlight energy variation, the concentration of oxygen can be obtained by loss value.
In the present invention, narrow band laser 1 is through fibre optic isolater 2 connecting fiber coupling mechanism, mainly eliminates the impact of reverse laser on narrow band laser, and its cardinal principle utilizes the one-way transmission of faraday's luminous effect realization to luminous energy, prevents reverse transfer.Flashlight detector 5 and reference light detector 11 all adopt silicon-based detector, realize the translation function of light signal to electric signal.The main medium connecting an optical element is general single mode fiber (SMF-28).Ammonia place is adopted after micro-nano fiber composite-structure film plating
reason is mainthe structural strength in order to strengthen superficial film of syllabus.
fig. 2for the signal of micro-nano fiber composite structure
figure,
fig. 3for
fig. 2in I-I partial enlargement
figure,
fig. 2,
fig. 3in, around micro-nano fiber 11, have one deck doping sol-gel films 12, doping collosol and gel particle 13 is one of particles in doping sol-gel films.
The laser that generating device of laser in the present invention sends is connected to micro-nano fiber composite structure sensing unit 4 through single-mode fiber, the change of doping sol-gel films physicochemical property is caused under different oxygen concentration, thus affect the transport property of micro-nano fiber composite structure, cause the change of luminous power.By the change of sensed light signal, the concentration of oxygen can be extrapolated.
fig. 4for automation mechanized operation program of the present invention, after initial step 100, judge whether 102 complete initialization.If response is affirmative, then step 104 input parameter, this output parameter comprises port selection, benchmark school zero etc., then step 106 obtains added losses value, eliminates the power jitter of generating device of laser itself mainly through flashlight detector testing result divided by reference light detector testing result.Speed up step 108 and input boundary condition and correlation parameter, comprise border acceptance condition, waveguide dimensions, material calculation etc., then step 110 obtains the relation between added losses and oxygen concentration.Finally start and export step 112, this output can be obtained in certain indicator, or be stored with other record that can retain this result.
Claims (4)
1. an oxygen monitoring device, it is characterized in that, described monitoring device comprises generating device of laser, 2 × 2 coupling mechanisms (3), micro-nano fiber composite structure sensing unit (4), flashlight detector (5), reference light detector (11), amplifier (6), difference engine (7), AD converter (8), phase locking modulator (9), microcomputer (10), and wherein generating device of laser contains narrow linewidth laser (1), fibre optic isolater (2); After the output terminal of described narrow linewidth laser (1) is connected to fibre optic isolater (2) by optical patchcord, connect the first port of 2 × 2 coupling mechanisms (3), 2 × 2 coupling mechanisms (3) the 3rd port is connected with flashlight detector (5) by micro-nano fiber composite structure sensing unit (4), and the 4th port of 2 × 2 coupling mechanisms (3) is connected with reference light detector (11) by optical fiber; Flashlight detector (5) is connected with amplifier (6), difference engine (7), AD converter (8), phase locking modulator (9), microcomputer (10) successively; Described narrow linewidth laser (1) is electrically connected with phase locking modulator (9), exports electric signal synchronous with the input electrical signal of generating device of laser for phase locking modulator (9); Described generating device of laser is by 2 × 2 coupling mechanisms, occurred laser is divided into two-way, the road that separates inputs to micro-nano fiber composite structure sensing unit (4), flashlight detector (5) successively as flashlight, and an other road is as the reference light detector (11) inputed to reference to light for detecting reference light intensity.
2. oxygen monitoring device according to claim 1, is characterized in that: described micro-nano fiber composite structure sensing unit (4) is made up of micro-nano fiber and the sol-gel chlorination tris (bipyridine) ruthenium potpourri that is coated on micro-nano fiber surface.
3. oxygen monitoring device according to claim 2, it is characterized in that: the diameter of described micro-nano fiber composite structure sensing unit (4) is 1 μm ~ 4 μm, the thickness being coated on the sol-gel chlorination tris (bipyridine) ruthenium potpourri clad on micro-nano fiber surface is 100nm ~ 200nm.
4. an oxygen monitoring method, is characterized in that, comprises the following steps successively:
A). be that the general single mode fiber SMF-28 of 125 microns utilizes scanning melting to draw cone farad to make the micro-nano fiber that diameter is 1 μm ~ 4 μm by diameter;
B). chlorination tris (bipyridine) ruthenium is dissolved in absolute ethyl alcohol according to the ratio of mass ratio 1:1 and obtains mixed solution, then mixed solution is mixed according to the ratio of volume ratio 1:50 with the sol gel solution of preparation, abundant stirring and dissolving;
C). by the micro-nano fiber drawn, utilize czochralski method plated film, thicknesses of layers 100nm ~ 200nm, and encapsulate, obtain oxygen micro-nano fiber composite structure sensing unit;
D). the laser occurred by generating device of laser connects micro-nano fiber composite structure as flashlight;
E). micro-nano fiber composite structure connects the flashlight detector being used for detection signal light intensity;
F). generating device of laser produces laser, the laser produced transfers to flashlight detector by micro-nano fiber composite structure, divided by reference light detector testing result, flashlight detector testing result show that the micro-nano fiber composite structure rete physicochemical property caused by oxygen concentration difference change and the light energy output variable quantity of generation;
G). utilize time-domain finite difference to obtain the concentration of oxygen according to the variable quantity of light energy output.
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| CN107014797A (en) * | 2017-06-15 | 2017-08-04 | 哈尔滨工业大学 | A kind of oxyty detection probe and its manufacture method |
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Application publication date: 20151230 |