CN109540326B - Fluorescence intensity ratio temperature measurement method based on dual-wavelength light source - Google Patents
Fluorescence intensity ratio temperature measurement method based on dual-wavelength light source Download PDFInfo
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Abstract
A fluorescence intensity ratio temperature measuring method based on a dual-wavelength light source,the invention relates to a fluorescence intensity ratio temperature measurement method based on a dual-wavelength light source. The invention aims to solve the problem that the relative sensitivity of the existing rare earth ion fluorescence intensity temperature measurement technology in a higher temperature range can be rapidly attenuated, and the invention records the rare earth Tb in the temperature range of 303 to 783K3+The ion is excited by a light source with the wavelength of 310nm and 378nm after the xenon lamp is subjected to light splitting, the central wavelength of the ion is in the intensity ratio of green fluorescence with the wavelength of 545nm, the functional relation between the intensity ratio and the temperature is a temperature measurement curve, and the temperature measurement curve can be used for measuring the temperature of an unknown environment. Based on the method, more sensitive temperature response can be obtained in a higher temperature range, the sensitivity is obviously superior to that of the conventional optical method, and the method is applied to the field of fluorescence intensity ratio temperature measurement.
Description
Technical Field
The invention relates to a fluorescence intensity ratio temperature measurement method based on a dual-wavelength light source.
Background
The importance of temperature is self-evident, and therefore how to obtain this parameter accurately and quickly becomes exceptionally critical. With the development of science and technology, temperature measurement methods are more and more diversified, wherein optical temperature measurement methods become more and more important, and because the methods can be applied to non-contact occasions and the response time is very short, the application scene of temperature measurement is greatly expanded.
Among the numerous optical thermometry methods, lanthanide-based fluorescence intensity ratio thermometry techniques have received much attention because of the following advantages: (1) because the temperature measurement is carried out by adopting a ratio method, the capacity of resisting external factors (such as the fluctuation of a laser light source and the loss of fluorescence transmission) is stronger; (2) the method has higher temperature measurement sensitivity, which also means that the method has better temperature resolution. It is worth noting that although the fluorescence intensity ratio based on lanthanide has higher relative thermometric sensitivity in the room temperature and low temperature region than the thermometric technique, the sensitivity attenuation amplitude is extremely large with the temperature rise, and the temperature resolution is also reduced, so that it is not suitable for characterizing the temperature in the higher temperature region.
Disclosure of Invention
The invention aims to solve the problem that the relative sensitivity of the existing rare earth ion fluorescence intensity temperature measurement technology in a higher temperature range can be rapidly attenuated, and provides a fluorescence intensity ratio temperature measurement method based on a dual-wavelength light source.
The invention relates to a fluorescence intensity ratio temperature measurement method based on a dual-wavelength light source, which is carried out according to the following steps: (1) preparation of CaWO4:Tb3+The temperature sensitive material is placed on a heating table, a 150W xenon lamp is used as an excitation light source, and a grating spectrometer is used as a light splitting instrument; (2) heating the heating table in a temperature range from 303K to 783K, wherein the temperature interval of each calibration temperature is 40K, irradiating the sample by using a light source with the center wavelength of 310nm of a split xenon lamp, and recording the Tb of rare earth3+The intensity of the green fluorescence emitted by the ion is recorded as fluorescence intensity A; irradiating the sample by using a light source with the center wavelength of 378nm of the xenon lamp subjected to light splitting, and recording rare earth Tb3+The intensity of green fluorescence emitted by the ions is recorded as fluorescence intensity B, and the ratio of the fluorescence intensity A to the fluorescence intensity B is obtained; (3) obtaining a fluorescence intensity ratio at each calibration temperature, obtaining a fitting curve after processing, obtaining a corresponding function relation R between the fluorescence intensity and the calibration temperature of 0.01 x exp (T/143) -0.07 according to the fitting curve, wherein R is rare earth Tb under the excitation of light sources with central wavelengths of 310nm and 378nm respectively3+The intensity ratio of the ion-emitted green fluorescence, T is the absolute temperature; (4) mixing CaWO4:Tb3+Placing the temperature sensitive material in an environment to be measured, and then placing CaWO4:Tb3+Rare earth Tb of temperature sensitive material under excitation of light sources with central wavelengths of 310nm and 378nm respectively3+Substituting the intensity ratio of the ion-emitted green fluorescence into the function to obtain the temperature of the environment to be measured, and completing the fluorescence intensity ratio temperature measurement method based on the dual-wavelength light source.
The invention utilizes two physical mechanisms with different temperature dependencies, and one mechanism enables the rare earth Tb to rise along with the rise of temperature3+The green fluorescence emitted by the ions is gradually enhanced, and the other mechanism causes the rare earth Tb3+The green fluorescence emitted by the ions is gradually reduced, so that the two opposite change laws ensure that the invention is based on the dual-wavelength light sourceThe fluorescence intensity ratio temperature measurement method can obtain higher temperature measurement sensitivity on the basis of the traditional lanthanide-based fluorescence intensity ratio temperature measurement technology.
The applicable temperature range of the invention is 303K to 783K, but the invention can be applied in a wider temperature range.
The invention has the beneficial effects that: besides the traditional lanthanide-based fluorescence intensity ratio temperature measurement technology, more choices are provided, more forms of ratio method temperature measurement can be carried out by using fluorescence, an optical temperature measurement method is beneficially supplemented, meanwhile, the relative sensitivity of the method is obviously superior to that of the conventional optical method, and the obtained relative sensitivity can reach 1.65 percent K at the temperature of 300K-1At 800K, 0.8% K can be reached-1. By contrast, the relative sensitivity of conventional optical methods at 300K is only 1.1% K-1The relative sensitivity at 800K is only 0.18% K-1Thus, the present invention provides a method and strategy for increasing the relative sensitivity of fluorescence ratio thermometry in higher temperature ranges.
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FIG. 1 shows a CaWO which is a temperature sensitive material of the present invention4:Tb3+The monitoring wavelength is 545 nm; wherein 1 is 303K, 2 is 343K, 3 is 383K, 4 is 423K, 5 is 463K, 6 is 503K, 7 is 543K, 8 is 583K, 9 is 623K, 10 is 663K, 11 is 703K, 12 is 743K, 13 is 783K;
FIG. 2 shows a CaWO which is a temperature sensitive material of the present invention4:Tb3+Variable temperature fluorescence spectroscopy, wherein the variable temperature interval is 303-783K, the variable temperature interval is 40K, and the excitation light source is a 310nm xenon light source subjected to light splitting;
FIG. 3 shows a CaWO which is a temperature sensitive material of the present invention4:Tb3+Variable temperature fluorescence spectroscopy, wherein the variable temperature interval is 303-783K, the variable temperature interval is 40K, and the excitation light source is a 378nm light-splitting xenon lamp light source;
FIG. 4 shows a CaWO which is a temperature sensitive material of the present invention4:Tb3+The change relationship between the fluorescence intensity ratio and the temperature under the excitation of the 310nm and 378nm light-splitting xenon lamp light sources; it is composed ofWherein c is a fitting curve, and d is a fluorescence intensity ratio;
FIG. 5 is a comparison of the relative sensitivity of a dual wavelength light source based fluorescence intensity ratio thermometry of the present invention versus the relative sensitivity of current conventional optical methods; where e is the relative sensitivity of the present example and f is the relative sensitivity of the conventional method.
Detailed Description
The first embodiment is as follows: the embodiment of the invention relates to a fluorescence intensity ratio temperature measurement method based on a dual-wavelength light source, which is carried out according to the following steps: (1) preparation of CaWO4:Tb3+The temperature sensitive material is placed on a heating table, a 150W xenon lamp is used as an excitation light source, and a grating spectrometer is used as a light splitting instrument; (2) heating the heating table in a temperature range from 303K to 783K, wherein the temperature interval of each calibration temperature is 40K, irradiating the sample by using a light source with the center wavelength of 310nm of a split xenon lamp, and recording the Tb of rare earth3+The intensity of the green fluorescence emitted by the ion is recorded as fluorescence intensity A; irradiating the sample by using a light source with the center wavelength of 378nm of the xenon lamp subjected to light splitting, and recording rare earth Tb3+The intensity of green fluorescence emitted by the ions is recorded as fluorescence intensity B, and the ratio of the fluorescence intensity A to the fluorescence intensity B is obtained; (3) obtaining a fluorescence intensity ratio at each calibration temperature, obtaining a fitting curve after processing, obtaining a corresponding function relation R between the fluorescence intensity and the calibration temperature of 0.01 x exp (T/143) -0.07 according to the fitting curve, wherein R is rare earth Tb under the excitation of light sources with central wavelengths of 310nm and 378nm respectively3+The intensity ratio of the ion-emitted green fluorescence, T is the absolute temperature; (4) mixing CaWO4:Tb3+Placing the temperature sensitive material in an environment to be measured, and then placing CaWO4:Tb3+Rare earth Tb of temperature sensitive material under excitation of light sources with central wavelengths of 310nm and 378nm respectively3+Substituting the intensity ratio of the ion-emitted green fluorescence into the function to obtain the temperature of the environment to be measured, and completing the fluorescence intensity ratio temperature measurement method based on the dual-wavelength light source.
The embodiment utilizes two physical mechanisms with different temperature dependencies and increases the temperatureA mechanism for making rare earth Tb3+The green fluorescence emitted by the ions is gradually enhanced, and the other mechanism causes the rare earth Tb3+The green fluorescence emitted by the ions is gradually reduced, so that the fluorescence intensity ratio temperature measurement method based on the dual-wavelength light source can obtain higher temperature measurement sensitivity on the basis of the traditional lanthanide-based fluorescence intensity ratio temperature measurement technology due to two opposite change rules.
The applicable temperature range of the present embodiment is 303K to 783K, but the present embodiment can be applied to a wider temperature range.
The beneficial effects of the embodiment are as follows: besides the traditional lanthanide-based fluorescence intensity ratio temperature measurement technology, more choices are provided, more forms of ratio method temperature measurement can be carried out by using fluorescence, an optical temperature measurement method is beneficially supplemented, meanwhile, the relative sensitivity of the method is obviously superior to that of the conventional optical method, and the obtained relative sensitivity can reach 1.65 percent K at the temperature of 300K-1At 800K, 0.8% K can be reached-1. By contrast, the relative sensitivity of conventional optical methods at 300K is only 1.1% K-1The relative sensitivity at 800K is only 0.18% K-1Thus, the present invention provides a method and strategy for increasing the relative sensitivity of fluorescence ratio thermometry in higher temperature ranges.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: CaWO4: Tb in step (1)3+The preparation method of the temperature sensitive material is a high-temperature solid phase method, the calcination temperature is 1150 ℃, and the heat preservation time is 6 hours. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: CaWO4: Tb prepared in step (1)3+Tb in temperature sensitive material3+Is 5 percent. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: and (3) the heating table stays at each calibration temperature for 2min in the step (2). The others are the same as in one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: and (4) obtaining a fitting curve by using a least square method principle in the step (3). The other is the same as one of the first to fourth embodiments.
The beneficial effects of the present invention are demonstrated by the following examples:
the first embodiment is as follows: the fluorescence intensity ratio temperature measurement method based on the dual-wavelength light source is carried out according to the following steps: (1) preparation of CaWO4:Tb3+The temperature sensitive material is placed on a heating table, a 150W xenon lamp is used as an excitation light source, and a grating spectrometer is used as a light splitting instrument; (2) heating the heating table in a temperature range from 303K to 783K, wherein the temperature interval of each calibration temperature is 40K, irradiating the sample by using a light source with the center wavelength of 310nm of a split xenon lamp, and recording the Tb of rare earth3+The intensity of the green fluorescence emitted by the ion is recorded as fluorescence intensity A; irradiating the sample by using a light source with the center wavelength of 378nm of the xenon lamp subjected to light splitting, and recording rare earth Tb3+The intensity of green fluorescence emitted by the ions is recorded as fluorescence intensity B, and the ratio of the fluorescence intensity A to the fluorescence intensity B is obtained; (3) obtaining a fluorescence intensity ratio at each calibration temperature, obtaining a fitting curve after processing, obtaining a corresponding function relation R between the fluorescence intensity and the calibration temperature of 0.01 x exp (T/143) -0.07 according to the fitting curve, wherein R is rare earth Tb under the excitation of light sources with central wavelengths of 310nm and 378nm respectively3+The intensity ratio of the ion-emitted green fluorescence, T is the absolute temperature; (4) mixing CaWO4:Tb3+Placing the temperature sensitive material in an environment to be measured, and placing CaWO4:Tb3+Rare earth Tb of temperature sensitive material under excitation of light sources with central wavelengths of 310nm and 378nm respectively3+Substituting the intensity ratio of the ion-emitted green fluorescence into the function to obtain the temperature of the environment to be measured, and completing the fluorescence intensity ratio temperature measurement method based on the dual-wavelength light source.
This example relates first to CaWO4:Tb3+Preparing temperature sensitive material by tabletting the weighed powderAnd (3) treating, namely preparing by adopting a traditional simple high-temperature solid phase method, wherein the calcining temperature is 1150 ℃, the heat preservation time is 6 hours, and then fixing the calcined fluorescent sheet into a groove of a heating table.
Rare earth Tb3+The main emission fluorescence band of the ions is located at 545nm, so that the monitoring wavelength is 545nm, and the temperature-varying excitation spectrum of the sample is obtained by changing the temperature of the sample in the temperature interval of 303 to 783K, and the result is shown in FIG. 1. It can be seen that the spectra at different wavelength positions show different trends with monotonic temperature increase, the fluorescence intensity at 310nm gradually increases with temperature increase, and the fluorescence intensity at 378nm gradually decreases with temperature increase, so that the sample is excited by the light sources at the two wavelengths.
Firstly, a xenon lamp is subjected to light splitting by using a grating spectrometer, the light splitting central wave band is 310nm, then the sample is irradiated by the xenon lamp after light splitting, the temperature of the sample is changed in a temperature interval from 303K to 783K to obtain the variable temperature emission fluorescence spectrum of the sample, and the result is shown in figure 2. It can be seen that the 545nm fluorescence peak is gradually increased with the monotonic increase of temperature, and the intensity of the fluorescence peak tends to decrease after the temperature is increased to 743K.
Then, a xenon lamp is subjected to light splitting by using a grating spectrometer, the light splitting center waveband is 378nm, then the sample is irradiated by the xenon lamp after light splitting, the temperature of the sample is changed in a temperature interval from 303K to 783K to obtain a temperature-variable emission fluorescence spectrum of the sample, and the result is shown in fig. 3. As can be seen, the 545nm fluorescence peak is gradually decreased with the monotonic increase in temperature.
The intensity of the 545nm fluorescence peak is obtained by integrating the area of the 545nm fluorescence peak, at each temperature, the corresponding fluorescence intensity ratio can be obtained by dividing the two intensities under the irradiation of a light source at 310nm and a light source at 378nm, so that 13 fluorescence intensity ratios can be obtained in the temperature interval from 303 to 783K, the change rule of the ratios along with the temperature is shown in FIG. 4, and it can be seen that the fluorescence intensity ratio monotonically increases along with the increase of the temperature, and the optimal fitting function can be obtained by fitting the data points: r is 0.01 ═ Cexp (T/143) -0.07, where R is rare earth Tb excited by light sources with central wavelengths of 310nm and 378nm3+The ion emits green fluorescence in intensity ratio, and T is absolute temperature.
Finally, this implementation tested the relative sensitivity according to the definition of relative sensitivity, as shown in FIG. 5, which also shows the relative sensitivity of the current conventional lanthanide-based fluorescence intensity vs. thermometry technique. The relative sensitivity obtained by the embodiment can reach 1.65 percent K at the temperature of 300K-1At 800K, 0.8% K can be reached-1. By contrast, the relative sensitivity of conventional optical methods at 300K is only 1.1% K-1The relative sensitivity at 800K is only 0.18% K-1It can be found that in the temperature range of room temperature and above, especially in the higher temperature region, the relative sensitivity of the method proposed by the present invention is significantly better than that of the conventional optical ratio temperature measurement technique, which also means that a higher temperature resolution can be obtained by using the method.
Claims (5)
1. A fluorescence intensity ratio temperature measurement method based on a dual-wavelength light source is characterized by comprising the following steps of: (1) preparation of CaWO4:Tb3+The temperature sensitive material is placed on a heating table, a 150W xenon lamp is used as an excitation light source, and a grating spectrometer is used as a light splitting instrument; (2) heating the heating table in a temperature range from 303K to 783K, wherein the temperature interval of each calibration temperature is 40K, irradiating the sample by using a light source with the center wavelength of 310nm of a split xenon lamp, and recording the Tb of rare earth3+The intensity of the green fluorescence emitted by the ion is recorded as fluorescence intensity A; irradiating the sample by using a light source with the center wavelength of 378nm of the xenon lamp subjected to light splitting, and recording rare earth Tb3+The intensity of green fluorescence emitted by the ions is recorded as fluorescence intensity B, and the ratio of the fluorescence intensity A to the fluorescence intensity B is obtained; (3) obtaining a fluorescence intensity ratio at each calibration temperature, obtaining a fitting curve after processing, obtaining a corresponding functional relation R between the fluorescence intensity and the calibration temperature of 0.01 × exp (T/143) -0.07 according to the fitting curve,wherein R is rare earth Tb excited by light sources with central wavelengths of 310nm and 378nm respectively3+The intensity ratio of the ion-emitted green fluorescence, T is the absolute temperature; (4) mixing CaWO4:Tb3+Placing the temperature sensitive material in an environment to be measured, and then placing CaWO4:Tb3+Rare earth Tb of temperature sensitive material under excitation of light sources with central wavelengths of 310nm and 378nm respectively3+Substituting the intensity ratio of the ion-emitted green fluorescence into the function to obtain the temperature of the environment to be measured, and completing the fluorescence intensity ratio temperature measurement method based on the dual-wavelength light source.
2. The method for measuring fluorescence intensity ratio of claim 1, wherein the step (1) is CaWO4: Tb3+The preparation method of the temperature sensitive material is a high-temperature solid phase method, the calcination temperature is 1150 ℃, and the heat preservation time is 6 hours.
3. The method for measuring fluorescence intensity ratio according to claim 1, wherein the CaWO4: Tb prepared in step (1)3+Tb in temperature sensitive material3+Is 5 percent.
4. The method of claim 1, wherein the heating stage stays at each calibration temperature for 2min in step (2).
5. The method of claim 1, wherein the step (3) is performed by using least squares to obtain the fitting curve.
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