CN102798485B - Temperature sensing method based on upconversion fluorescent powder - Google Patents
Temperature sensing method based on upconversion fluorescent powder Download PDFInfo
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- CN102798485B CN102798485B CN201210288592.2A CN201210288592A CN102798485B CN 102798485 B CN102798485 B CN 102798485B CN 201210288592 A CN201210288592 A CN 201210288592A CN 102798485 B CN102798485 B CN 102798485B
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Abstract
The invention relates to a temperature sensing method based on upconversion fluorescent powder. The temperature sensing method based on upconversion fluorescent powder comprises the following steps that: (1) one end of a fluorescent powder bar is adhered to the common end of Y-shaped multimode fiber and is fixed in a semi-closed light-transmitting tube, and the other end of the fluorescent powder bar serves as a temperature sensing head and is arranged at the closed end of the light-transmitting tube; and one end of the forked end of the Y-shaped multimode fiber is connected with a light source and the other end of the forked end of the Y-shaped multimode fiber is connected with a spectrometer; 2) the closed end of the light-transmitting end serves as a temperature sensing head and is placed in an object to be measured; and 3) after outgoing, the light rays of the light source enter one end of the forked end of the Y-shaped multimode fiber and excite the fluorescent powder bar; the excited fluorescent is led out of the other end of the forked end of the Y-shaped multimode fiber and detected by the spectrometer; the corresponding optical spectrum is transmitted to a computer; and calibration is performed according to the corresponding relationship between fluorescence intensity ratio and temperature, so that the actually measured temperature value is output. Fluorescent powder is doped in light-transmitting glue, so the sensor has higher sensitivity, wider temperature-measuring range and higher temperature stability.
Description
Technical field
The present invention relates to a kind of fiber-sensing measuring method, more particularly, relate to a kind of temperature sensing method based on up-conversion phosphor.
Background technology
Fibre optic temperature sensor is high with its precision, sensing scope is wide, be not subject to the advantages such as electromagnetic interference (EMI), has been widely used in the fields such as intelligent grid, biologic medical, petrochemical complex, industrial microwave, power management and military and national defense.Especially, the fluorescent optical fiber temperature sensor of utilizing pure optical principle to carry out parameter measurement has the incomparable advantage of traditional sensing technology and the researchists' that are subject to getting more and more concern.Although some fluorescent optical fiber temperature sensor have realized small serial production on market, along with the continuous expansion of application, the fluorescent material of superior performance continues to bring out, and the design of sensor is faced with new opportunities and challenges.
The advantage of fluorescence intensity ratio fibre optic temperature sensor maximum is that heat transfer agent depends on the variation of strength ratio, is not subject to the impact of the factors such as light source fluctuation, fiber transmission attenuation, junction loss.At present, about adopting fluorescence intensity ratio to carry out thermometric research, major part concentrates on rare-earth doped optical fibre, less for the report of some other rare earth luminescent materials such as fluorescent powder.Such as the people such as Kusama ([1] Kusama, H., O.J.Sovers, T.Y oshioka.Line shif method for phosphortemperature measurements.Japanese Journal ofApplied Physics, 1996,15 (12): 2345) studied employing Y
2o
2s:Eu
3+the beam intensity ratio that two different excited state transition of fluorophor obtain is carried out optical fiber sensing measurement; ([2] Bai Haiying of department of physics of Northwestern Polytechnical University, Wang Jimin. the fluorescent optical fiber temperature sensor system [J] based on novel rare-earth luminescent material. sensing technology journal, 2004, (4): 660-662) designed a set of fluorescence fiber temperature measurement system based on rare-earth luminescent material.System is with rare earth material Y
2o
2s:Eu+Fe
2o
3as sensitive material, temperature-measuring range is 25 ~ 85 ℃.These two kinds of thermometric schemes all because of the lower thermal quenching temperature limiting of material self temperature-measuring range of temperature sensor, and there is complex process, high in cost of production shortcoming.Meanwhile, the peak emission wavelength of this two classes fluorescent material only has two, and when the fluorescence of different peak wavelengths calculates its strength ratio, dirigibility is limited to, and has the defects such as sensitivity is lower.
For up-conversion phosphor material property, stablize, easily synthesize, can greatly reduce the cost of manufacture of sensor.Therefore research can utilize the advantage of Fibre Optical Sensor, can not introduce complicated system again, uses low cost, the high performance novel optical fiber fluorescence temperature sensor of ordinary light source, fluorescent material, detector etc. to be significant.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of fluorescence intensity ratio, experimental facilities of measuring different wave length under the pumping of Same Wavelength light source small and exquisite easy, cost of manufacture is low, highly sensitive, temperature-measuring range is wide, cost is low, temperature stability the is good temperature sensing method based on up-conversion phosphor.
Technical scheme of the present invention is as follows:
A temperature sensing method based on up-conversion phosphor, comprises light source, optical fiber, up-conversion phosphor, spectrometer, light-transmission tube; Described up-conversion phosphor is entrained in printing opacity glue, is the structure of fluorescent powder rod; Described light-transmission tube is semiclosed light-transmission tube; Described optical fiber is Y type multimode optical fiber;
Step is as follows:
1), described fluorescent powder rod one end is mutually bonding with the common port of Y type multimode optical fiber, is fixed in semi-enclosed light-transmission tube, the other end, as Temperature probe, is arranged at the blind end place of light-transmission tube; One end of the divergent ends of Y type multimode optical fiber is connected with light source, and the other end of divergent ends is connected with spectrometer;
2), the blind end of light-transmission tube is as Temperature probe, is placed in object under test;
3), after the beam projecting of light source, enter one end of the divergent ends of Y type multimode optical fiber, activating fluorescent Powder Rod, the fluorescence exciting is derived from the other end of the divergent ends of Y type multimode optical fiber, by spectrometer detect and by corresponding spectral transmissions to computing machine, according to the corresponding relation of fluorescence intensity ratio and temperature, calibrate, thus the temperature value of output actual measurement.
As preferably, between one end of the divergent ends of light source and Y type multimode optical fiber, be provided with coupled lens.
As preferably, described up-conversion phosphor is NaYF
4: Yb
3+/ Er
3+up-conversion phosphor.
As preferably, described light source is 980nm pump laser.
As preferably, described light-transmission tube is quartz ampoule.
As preferably, the response wave length scope of described its detector of spectrometer is at 200 ~ 1100nm.
The adulterate preparation method of fluorescent powder rod of up-conversion phosphor, step is as follows:
A), get the NaYF of equal proportion
4: Yb
3+/ Er
3+fluorescent powder, Powdered healant, gluey healant;
B), by NaYF
4: Yb
3+/ Er
3+fluorescent powder, Powdered healant are placed in mortar and fully grind;
C), again add gluey healant to carry out regrind, the semi-solid pasty state of furnishing;
D), semi-solid pasty state is made to club shaped structure.
As preferably, further comprise:
E), by step D) club shaped structure making is adhered to the common port of Y type multimode optical fiber, is fixed on the blind end of semi-enclosed light-transmission tube;
F), at normal temperatures solidify the constant temperature oven 2 hours place 80 ℃ after 16 hours, be after this slowly warming up to 150 ℃ and keep 2 hours, slowly cool to room temperature and complete curing.
Beneficial effect of the present invention is as follows:
Adopt technical solutions according to the invention, adopt up-conversion phosphor to make, based on most up-conversion phosphors, under certain wavelength pumping, having a plurality of peak emission wavelengths, while therefore selecting the fluorescence of different peak wavelengths to calculate its strength ratio, there is larger dirigibility; Meanwhile, the 900 ~ 1000nm wave band light source cost that is used in pumping due to the development of optical fiber communication is lower, is easy to obtain, and pump light and emitting fluorescence wavelength interval are far away in addition, is easy to realize filtering and eliminates the adverse effect of pump light to fluoroscopic examination.
Adopt up-conversion phosphor, under the pumping of Same Wavelength light source, measure the fluorescence intensity ratio of different wave length.The method can overcome most fluorescent materials and only have single emission peak, cannot realize the difficult problem that different wave length fluorescence intensity ratio is measured.
The present invention is entrained in fluorescent powder in printing opacity glue, makes that sensor overall sensitivity is higher, temperature-measuring range is wider, temperature stability is better.
Accompanying drawing explanation
Fig. 1 is the connection diagram based on experiment measuring of the present invention;
Fig. 2 measures resulting spectroscopic temperature performance plot based on low temperature test of the present invention;
Fig. 3 is based on the resulting spectroscopic temperature performance plot of high temperature experiment measuring of the present invention;
Fig. 4 is based on the resulting Er of experiment measuring of the present invention
3+the different energy level fluorescent emission of ion peak value varies with temperature curve map;
Fig. 5 is based on the resulting fluorescence intensity ratio I of experiment measuring of the present invention
519nm/ I
539nmwith I
519nm/ I
653nmtemperature characteristics figure;
In figure: the 1st, light source, the 2nd, Y type multimode optical fiber, the 3rd, spectrometer, the 4th, light-transmission tube, the 7th, fluorescent powder rod, the 8th, computing machine, the 9th, temperature controller, the 10th, cabinet-type electric furnace.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
A temperature sensing method based on up-conversion phosphor, as shown in Figure 1, experimental facilities comprises light source 1, optical fiber, fluorescent powder rod 7, spectrometer 3, semi-enclosed light-transmission tube 4, computing machine 8, temperature controller 9, cabinet-type electric furnace 10.
Step is as follows:
1), described fluorescent powder rod 7 one end are mutually bonding with the common port of Y type multimode optical fiber 2, are fixed in semi-enclosed light-transmission tube 4, the other end, as Temperature probe, is arranged at the blind end place of light-transmission tube 4; One end of the divergent ends of Y type multimode optical fiber 2 is connected with light source 1, and the other end of divergent ends is connected with spectrometer 3; Between one end of the divergent ends of light source 1 and Y type multimode optical fiber 2, be provided with coupled lens.Spectrometer 3 is connected with the other end of the divergent ends of Y type multimode optical fiber 2.
2), the blind end of light-transmission tube 4 is as Temperature probe, is placed in object under test;
3), after the beam projecting of light source 1, enter one end of the divergent ends of Y type multimode optical fiber 2, activating fluorescent Powder Rod 7, the fluorescence exciting is derived from the other end of the divergent ends of Y type multimode optical fiber 2, by spectrometer 3 detect and by corresponding spectral transmissions to computing machine 8, according to the corresponding relation of fluorescence intensity ratio and temperature, calibrate, thus the temperature value of output actual measurement.
In the present embodiment, in described fluorescent powder rod 7, doped with up-conversion phosphor, described semiclosed light-transmission tube 4 is quartz ampoule, and described optical fiber is Y type multimode optical fiber 2.Described up-conversion phosphor is NaYF
4: Yb
3+/ Er
3+up-conversion phosphor; Described light source 1 is 980nm pump laser.
Doping NaYF
4: Yb
3+/ Er
3+fluorescent powder rod 7 one end of up-conversion phosphor are as Temperature probe, and the other end is mutually bonding with the common port of Y type multimode optical fiber 2, is fixed in semi-enclosed quartz ampoule.980nm pump light source enters one end de-energisation NaYF of the divergent ends of Y type multimode optical fiber 2 after coupled lens coupling
4: Yb
3+/ Er
3+up-conversion fluorescence powder rod 7, the fluorescence exciting is derived from the other end of the divergent ends of Y type multimode optical fiber 2, by micro spectrometer 3 detect and by corresponding spectral transmissions to computing machine 8, according to the corresponding relation of fluorescence intensity ratio and temperature, calibrate, thus the temperature value of output actual measurement.
In the present embodiment, adopt the experimental provision shown in Fig. 1, tested NaYF at 25 ~ 180 ℃ of temperature
4: Yb
3+/ Er
3+fluorescent powder is in the fluorescence intensity of 500 ~ 700nm wave band.
Experimental result as shown in Figure 2 and Figure 3, three curves in Fig. 2, from top to bottom, the spectroscopic temperature performance plot while representing respectively 30 ℃, 50 ℃, 70 ℃.Five curves in Fig. 3, from top to bottom, the spectroscopic temperature performance plot while representing respectively 90 ℃, 110 ℃, 130 ℃, 150 ℃, 170 ℃.As can be seen from the figure,, when temperature rises to 170 ℃ from 30 ℃, the centre wavelength at the upper switching emission of 523nm, 537nm and 655nm peak does not change.
In conjunction with Fig. 4, analyze the variation with temperature situation of each emission peak: three curves in Fig. 4, starting point curve from top to bottom, represents that respectively the fluorescence intensity of 523nm, 537nm, 655nm emission peak varies with temperature curve map.As shown in Figure 4, the fluorescence intensity at 523nm place is along with the rising of temperature is gently fallen after rising, the fluorescence intensity of these two emission peaks of 537nm and 655nm reduces along with the rising of temperature, there is obvious dull downtrending, wherein the rate of change of 537nm curve is maximum, and 655nm curve declines comparatively mild.
When the method for employing fluorescence intensity ratio is carried out temperature detection, in two optimal situations of wave band selecting: the fluorescence intensity of a wave band is along with temperature raises and strengthens, the fluorescence intensity of another wave band is along with temperature raises and weakens, and the temperature control of fluorescence intensity ratio is higher like this.Fig. 5 is in 25 ~ 180 ℃ of temperature ranges, and two curves in figure,, represent respectively I from top to bottom
523nm/ I
655nmwith I
523nm/ I
537nmthe temperature variant family curve of ratio of two groups of fluorescence intensities.Fluorescence intensity linear fit when the solid line in figure is partly 32 temperature that record according to experiment.By I
523nm/ I
537nmcurve linear related coefficient K (I
519nm/ I
539nm)=0.9996 and I
523nm/ I
655nmcurve K (I
519nm/ I
653nm)=0.9993 is known, and the ratio of fluorescence intensity is that approximately linear changes with temperature, and I
523nm/ I
537nmcurve compares I
523nm/ I
655nmcurve approaches straight line more.From figure, can read intuitively the sensitivity of two
i
523nm/ I
537nmcurve (R (I
523nm/ I
537nm)-T) sensitivity is 0.005 ℃
-1, and I
523nm/ I
655nmcurve (R (I
523nm/ I
655nm)-T) sensitivity is 0.006 ℃
-1, be I
523nm/ I
537nm1.2 times of curve, embody higher sensitivity of thermometry advantage thus.
The present invention is based on most up-conversion phosphors and there are a plurality of emission peaks, when the fluorescence of selecting different peak wavelengths carries out strength ratio, there is larger dirigibility.Simultaneously, the relative visible light source of 900 ~ 1000nm wave band optical fiber coupling light source for pumping easily obtains, and due to pump light and emitting fluorescence wavelength interval far away, be easy to realize filtering and eliminate the impact of pump light on fluoroscopic examination, proposing the fluorescence intensity ratio temperature sensing method based on up-conversion phosphor.
The adulterate preparation method of fluorescent powder rod of up-conversion phosphor, step is as follows:
A), get the NaYF of equal proportion
4: Yb
3+/ Er
3+fluorescent powder, Powdered healant, gluey healant;
B), by NaYF
4: Yb
3+/ Er
3+fluorescent powder, Powdered healant are placed in mortar and fully grind;
C), again add gluey healant to carry out regrind, the semi-solid pasty state of furnishing;
D), semi-solid pasty state is made to club shaped structure;
E), by step D) club shaped structure making is adhered to the common port of Y type multimode optical fiber, is fixed on the blind end of semi-enclosed light-transmission tube;
F), at normal temperatures solidify the constant temperature oven 2 hours place 80 ℃ after 16 hours, be after this slowly warming up to 150 ℃ and keep 2 hours, slowly cool to room temperature and complete curing.
In the present embodiment, step is specific as follows: doping NaYF
4: Yb
3+/ Er
3+the preparation process of fluorescent powder rod is as follows: the NaYF that takes equal proportion with analytical balance
4: Yb
3+/ Er
3+fluorescent powder, Powdered healant and gluey healant.Under clean environment by NaYF
4: Yb
3+/ Er
3+being placed in mortar with two kinds of powder of Powdered healant fully grinds, add again gluey healant to carry out regrind, it is that 2mm height is the club shaped structure of 7mm that the semi-solid pasty state of furnishing is made to diameter, be adhered to the output terminal of Y type multimode optical fiber, be fixed on the blind end of internal diameter 2.5cm, the long quartz ampoule for 20cm.Solidify at normal temperatures the constant temperature oven 2 hours place 80 ℃ after 16 hours, be after this slowly warming up to 150 ℃ and keep 2 hours, slowly cool to room temperature, fluorescent powder rod completes curing.
Described healant is superhigh temperature healant, the HT-767 (A type) that Shi You Huitian Glue Ind Co., Ltd., Hubei produces.The polymer/metallic that described healant is comprised of metal, pottery, quartz, fiber, high-ductility heat stable resin and hardening agent, the bicomponent material of polymer-ceramic class form a kind of wear-resistant, corrosion-resistant, shock proof high polymer alloy and ceramic coat by chemical reaction after two components are fully mixed.
By research, find, most of rare-earth luminescent material, fiber optic materials, as before sensor, need to be heat-treated, to guarantee repeatability and the stability of sensor.After bakingout process, the measuring accuracy of sensor and sensitivity also can improve, but to different rare-earth luminescent materials, because of the maximum operating temperature difference that can bear, its corresponding heat treated maximum temperature should be set near its maximum operating temperature, otherwise material sharply fails because of impaired its fluorescent characteristic that makes.NaYF
4: Yb
3+/ Er
3+fluorescent powder rod adopts hydro-thermal method to be prepared, the maximum temperature of reaction is at 180 ℃, therefore the heat treatment process of this experiment is by the quartz ampoule with fluorescent powder rod and Y type multimode optical fiber preparing, be placed in constant temperature oven, by room temperature, slowly rise to 180 ℃ and keep 8 hours, to guarantee NaYF
4: Yb
3+/ Er
3+repeatability and stability.
Above-described embodiment is only for the present invention is described, and not as limitation of the invention.So long as according to technical spirit of the present invention, to above-described embodiment change, modification etc. all will drop in the scope of claim of the present invention.
Claims (7)
1. the temperature sensing method based on up-conversion phosphor, is characterized in that, comprises light source, optical fiber, fluorescent powder rod, spectrometer, light-transmission tube; Described light-transmission tube is semiclosed light-transmission tube; Described optical fiber is Y type multimode optical fiber;
Step is as follows:
1), described fluorescent powder rod one end is mutually bonding with the common port of Y type multimode optical fiber, is fixed in semi-enclosed light-transmission tube, the other end, as Temperature probe, is arranged at the blind end place of light-transmission tube; One end of the divergent ends of Y type multimode optical fiber is connected with light source, and the other end of divergent ends is connected with spectrometer;
2), the blind end of light-transmission tube is as Temperature probe, is placed in object under test;
3), after the beam projecting of light source, enter one end of the divergent ends of Y type multimode optical fiber, activating fluorescent Powder Rod, the fluorescence exciting is derived from the other end of the divergent ends of Y type multimode optical fiber, by spectrometer detect and by corresponding spectral transmissions to computing machine, according to the corresponding relation of fluorescence intensity ratio and temperature, calibrate, thus the temperature value of output actual measurement;
Wherein, the preparation method's of described fluorescent powder rod step is as follows:
A), get the NaYF of equal proportion
4: Yb
3+/ Er
3+fluorescent powder, Powdered healant, gluey healant;
B), by NaYF
4: Yb
3+/ Er
3+fluorescent powder, Powdered healant are placed in mortar and fully grind;
C), again add gluey healant to carry out regrind, the semi-solid pasty state of furnishing;
D), semi-solid pasty state is made to club shaped structure.
2. the temperature sensing method based on up-conversion phosphor according to claim 1, is characterized in that, between one end of the divergent ends of light source and Y type multimode optical fiber, is provided with coupled lens.
3. the temperature sensing method based on up-conversion phosphor according to claim 1, is characterized in that, described light source is 980nm pump laser.
4. the temperature sensing method based on up-conversion phosphor according to claim 1, is characterized in that, described light-transmission tube is quartz ampoule.
5. the temperature sensing method based on up-conversion phosphor according to claim 1, is characterized in that, the response wave length scope of described its detector of spectrometer is at 200～1100nm.
6. the adulterate preparation method of fluorescent powder rod of up-conversion phosphor, is characterized in that, step is as follows:
A), get the NaYF of equal proportion
4: Yb
3+/ Er
3+fluorescent powder, Powdered healant, gluey healant;
B), by NaYF
4: Yb
3+/ Er
3+fluorescent powder, Powdered healant are placed in mortar and fully grind;
C), again add gluey healant to carry out regrind, the semi-solid pasty state of furnishing;
D), semi-solid pasty state is made to club shaped structure.
7. the preparation method of the fluorescent powder rod of doping up-conversion phosphor according to claim 6, is characterized in that, further comprises:
E), by step D) club shaped structure making is adhered to the common port of Y type multimode optical fiber, is fixed on the blind end of semi-enclosed light-transmission tube;
F), at normal temperatures solidify the constant temperature oven 2 hours place 80 ℃ after 16 hours, be after this slowly warming up to 150 ℃ and keep 2 hours, slowly cool to room temperature and complete curing.
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