CN113881434B - Rare earth Dy (Dy) 3+ Ratio type temperature detection method for ion luminescence - Google Patents
Rare earth Dy (Dy) 3+ Ratio type temperature detection method for ion luminescence Download PDFInfo
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- 238000009529 body temperature measurement Methods 0.000 abstract description 21
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 19
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Abstract
Rare earth-based Dy 3+ The invention relates to a ratio type temperature detection method of ion luminescence, which adopts rare earth Dy 3+ Ionic thermal coupling energy level 4 I 15/2 And 4 F 9/2 respectively to the ground state 6 H 13/2 And metastable state 6 H 13/2 Blue and yellow up-conversion or down-conversion luminescence generated by energy level transition, and realizes rare earth-based Dy through quantitative relation between luminous intensity ratio of the two and temperature 3+ A new method of ion luminescence ratio type thermometry. Compared with the prior conventional Dy-based method 3+ The temperature measurement method of the ion two-blue down-conversion luminous intensity ratio can effectively avoid the problem of low luminous intensity measurement precision caused by the overlapping of two blue light luminous peaks, expands the temperature detection range of a lower temperature interval, and Dy 3+ The up-conversion luminescence and the down-conversion luminescence of the ions can be used for temperature detection, and the temperature detection sensitivity is greatly improved.
Description
Technical Field
The invention relates to a temperature detection method, in particular to a rare earth Dy 3+ The temperature detection method of the ion blue and yellow down-conversion or up-conversion luminescence intensity ratio.
Background
Temperature is a basic and very important thermodynamic state parameter, and the measurement of temperature occupies an extremely important position for social production, people's life and scientific research. The traditional contact type temperature measurement technology faces huge limitation, and the non-contact type temperature measurement technology avoids the damage of the measured medium to the temperature detection component because the temperature detection unit is not in direct contact with the measured medium, so that the non-contact type temperature measurement technology has wider application value. The fluorescence temperature detection technology has the advantages of strong anti-interference capability, high sensitivity and spatial resolution, quick response and the like, and becomes a hotspot of temperature measurement research in recent years. The fluorescence temperature detection technology uses fluorescent material as temperature detection medium and detects various fluorescence spectroscopyThe temperature measurement is realized by the change of parameters with the temperature, and the parameters comprise the position, the intensity, the half-peak width, the service life, the fluorescence intensity ratio and the like of the fluorescence peak sensitive to the temperature. The sensitivity of these spectroscopic parameters to temperature is often based on different temperature sensitive mechanisms. The method can eliminate the interference of non-temperature factors such as fluorescence loss, excitation light source power fluctuation, the number of luminescent centers and the like in the temperature measurement process, has the characteristics of small external interference, strong excitation power noise resistance and the like, and is the research focus of the current fluorescence temperature measurement technology. A plurality of rare earth ions having thermally coupled energy levels, e.g. Er 3+ : 2 H 11/2 / 4 S 3/2 、Tm 3+ : 3 F 2,3 / 3 H 4 、Ho 3 + : 5 S 2 / 5 F 4 、Nd 3+ : 4 F 5/2 / 4 F 3/2 、Dy 3+ : 4 I 15/2 / 4 F 9/2 And Eu 3+ : 5 D 1 / 5 D 0 Etc. are widely used for fluorescence intensity-versus-temperature detection. Wherein the rare earth Dy 3+ Thermally coupled energy levels of ions 4 I 15/2 And 4 F 9/2 the energy level difference is about 1200cm -1 And can generate bright blue light and yellow light emission under the excitation of ultraviolet light, so Dy 3+ Ions are also widely used to enable temperature measurement based on fluorescence intensity ratio.
At present, based on rare earth Dy 3+ The method for detecting temperature by ion luminescence mainly adopts Dy 3+ Two thermally coupled energy levels of ions 4 I 15/2 And 4 F 9/2 respectively to the ground state 6 H 15/2 Two blue light intensities (respectively marked as I) with central wavelengths emitted by energy level transition and located around 450 and 480nm Blue light I And I Blue light II ) Of ratio of (A) to (B) and temperatureQuantitative relationship therebetween. FIG. 1 shows rare earth Dy 3+ The energy level structure of the ion and the mechanism of light emission.
From Dy in FIG. 1 3+ Two thermally coupled energy levels of ions 4 I 15/2 And 4 F 9/2 respectively to the ground state 6 H 15/2 Luminous intensity I generated by energy level transition Blue light I And I Blue light II Can be respectively expressed as:
I blue light I ＝N 3 ω 30 g 30 hν 30 (1)
I Blue light II ＝N 2 ω 20 g 20 hν 20 (2)
Wherein N is 3 Are thermally coupled energy levels 4 I 15/2 The number of particles above;
N 2 are thermally coupled energy levels 4 F 9/2 The number of particles above;
ω 30 are thermally coupled energy levels 4 I 15/2 To the ground state 6 H 15/2 Spontaneous emission rate of energy level transition;
ω 20 are thermally coupled energy levels 4 F 9/2 To the ground state 6 H 15/2 Spontaneous emission rate of energy level transition;
g 30 are thermally coupled energy levels 4 I 15/2 To the ground state 6 H 15/2 Energy level degeneracy of the energy level transition;
g 20 are thermally coupled energy levels 4 F 9/2 To the ground state 6 H 15/2 Energy level degeneracy of the energy level transition;
ν 30 are thermally coupled energy levels 4 I 15/2 To the ground state 6 H 15/2 The light emission frequency of the energy level transition;
ν 20 are thermally coupled energy levels 4 F 9/2 To the ground state 6 H 15/2 The frequency of light emission of the energy level transition.
Thermally coupled energy level pair 4 I 15/2 And 4 F 9/2 number of particles N 3 And N 2 Satisfy a Boltzmann-type distribution, i.e.
Where Δ E is the energy difference between the two thermally coupled energy levels, k is the Boltzmann constant, and T is the absolute temperature. Thus coming from thermally coupled energy level pairs 4 I 15/2 And 4 F 9/2 to the ground state 6 H 15/2 Ratio of two blue light intensities generated by energy level transition (I) Blue light I /I Blue light II ) Can be expressed as:
wherein C is a constant related to the frequency of emitted light, the degree of degeneracy of the energy level, and the frequency of emitted light. According to the definition of the sensitivity of temperature detection, the absolute temperature sensitivity S a Can be expressed as:
at present, a great deal of literature reports different rare earth Dy 3+ Rare earth Dy based in ion-doped luminescent material 3+ Temperature sensing of ion-two blue luminous intensity ratio, e.g. Dy 3+ Doping with Y 4 Al 2 O 9 Fluorescent powder and Dy 3+ BaYF doping 5 Phosphor and Dy 3+ GdVO doping 4 Film, dy 3+ Gd-doped alloy 2 Ti 2 O 7 Phosphor and Dy 3+ Doping with Y 2 SiO 5 Phosphor and Dy 3+ Doped CaWO 4 Dy is observed in the fluorescent powder 3+ Ion I Blue light I /I Blue light II The quantitative relationship with temperature, dy-based was studied 3+ Ion I Blue light I /I Blue light II Intensity ratio temperature sensing behavior.
In addition, except for using Dy 3+ Ion intensity ratio of two blue lights for temperature detection, and Dy 3+ The temperature detection is carried out according to the change relation of the luminous intensity ratio of other wave bands of the ions along with the temperature. For example, dy 3+ Doping BaYF 5 Dy is built in the fluorescent powder 3+ Ion(s) 4 I 15/2 → 6 H 15/2 Blue luminescence and luminescence of transitions 4 F 9/2 → 6 H 11/2 Intensity ratio between red luminescence of transitions versus temperature; dy 3+ Gd-doped 2 Ti 2 O 7 Gd is adopted in the fluorescent powder 2 Ti 2 O 7 Trap luminescence and Dy of host 3+ Ion(s) 4 F 9/2 → 6 H 15/2 Sensing the temperature by the intensity ratio between the blue luminescence of the transition; dy (Dy) 3+ Doped CaWO 4 Dy is also explored in the fluorescent powder 3+ Ion(s) 4 G 11/2 → 6 H 15/2 Ultraviolet luminescence of transitions and 4 F 9/2 → 6 H 15/2 intensity ratio between blue luminescence of transitions versus temperature.
Due to Dy 3+ Ion thermal coupling energy level pair 4 I 15/2 And 4 F 9/2 the difference in energy levels between is about 1200cm -1 Cause to cause 4 I 15/2 → 6 H 15/2 And 4 F 9/2 → 6 H 15/2 the two blue luminescence peaks corresponding to the transitions are overlapped to a large extent, so Dy-based luminescence peaks are widely researched in the conventional art 3+ In the temperature measurement technology of the intensity ratio of two blue lights, the luminous intensity (i.e. I) of the two blue lights Blue light I And I Blue light II ) It is often difficult to measure accurately, so that the ratio of the luminous intensities (I) of the two blue lights Blue light I /I Blue light II ) There is a large error, resulting in a luminous intensity ratio (I) Blue light I /I Blue light II ) The relationship with temperature (T) deviates from the theoretical model of equation (4), reducing the accuracy of temperature sensing. For example in Dy 3+ Doping with Y 4 Al 2 O 9 Phosphor and Dy 3+ Gd-doped 2 Ti 2 O 7 FluorescencePowder and Dy 3+ Doping with Y 2 SiO 5 Dy exists in the fluorescent powder 3+ The two blue luminous peaks of the ion are overlapped to a large extent.
Furthermore, due to thermal coupling energy levels 4 I 15/2 And 4 F 9/2 follows the Boltzmann distribution, thermally coupling higher levels of energy levels at lower temperatures 4 I 15/2 Too little relative population of 4 I 15/2 → 6 H 15/2 The transition probability is low and no effective luminous intensity (i.e. I) can be obtained Blue light I ) Resulting in I at low temperature Blue light I /I Blue light II The ratio is also so small that I cannot be established at low temperatures Blue light I /I Blue light II Ratio-temperature relationship, and thus conventional Dy-based 3+ Method for measuring the ratio of two blue light intensities (i.e. I) Blue light I /I Blue light II ) Not suitable for lower temperature measurements. For example in Dy 3+ Doping with Y 4 Al 2 O 9 Fluorescent powder and Dy 3+ BaYF doping 5 Phosphor and Dy 3+ GdVO doping 4 Film, dy 3+ Doping with Y 2 SiO 5 Phosphor and Dy 3+ Doped CaWO 4 In the fluorescent powder, I exists in the low-temperature range of respective research Blue light I The intensity is too low, and thus, the method is not suitable for temperature detection in a lower temperature range.
Thirdly, regarding utilization of Dy 3+ In the investigation of temperature detection of the intensity ratio of luminescence in other wavelength bands of ions in relation to temperature, e.g. Dy 3+ Doping BaYF 5 Fluorescent powder and Dy 3+ Gd-doped alloy 2 Ti 2 O 7 Phosphor and Dy 3+ Doped CaWO 4 Fluorescent powder and the like, and the pure mathematical relationship between the luminous intensity ratio and the temperature is established by adopting empirical formulas. These established empirical formulas of luminescence intensity ratio versus temperature lack Dy 3+ The intrinsic physical mechanism between the luminous intensity ratio of ions and the temperature is only applicable to respective Dy studied 3+ Doped luminescent material systems have no universality.
Disclosure of Invention
The invention overcomes the defect that Dy based on rare earth in the prior art 3+ The defects of low luminous intensity measurement precision, poor low-temperature detection effect and low temperature sensitivity caused by the overlapping of luminous peaks in the ion two blue light intensity ratio temperature measurement technology are utilized by utilizing Dy 3+ The blue and yellow luminescence of the ion realizes a Dy-based luminescence by the quantitative relation between the intensity ratio of the luminescence of the blue and yellow luminescence and the temperature 3+ The novel ion-luminescence ratio-type temperature measurement method not only effectively avoids the problem of low luminous intensity measurement precision caused by the overlapping of luminous peaks, but also can effectively expand the temperature measurement range and improve the temperature detection sensitivity.
In order to achieve the purpose, the technical scheme of the invention is as follows: based on rare earth Dy 3+ Ion-doped luminescent material with ultraviolet or red light as excitation source to obtain light from Dy 3+ The blue and yellow down-conversion or up-conversion luminescence of (1) and temperature detection is performed based on the quantitative relationship between the blue and yellow luminescence intensity ratio and temperature. The quantitative relationship is as follows:
Dy 3+ two thermally coupled energy levels of ions 4 I 15/2 And 4 F 9/2 in addition to being able to move to the ground state 6 H 15/2 The energy level transition produces blue luminescence, and can also be converted into metastable state 6 H 13/2 The energy level transition produces a yellow emission whose yellow light intensity can be expressed as:
I Yellow light ＝N 3 ω 31 g 31 hν 31 +N 2 ω 21 g 21 hν 21 (6)
wherein N is 3 Are thermally coupled energy levels 4 I 15/2 The number of particles above;
N 2 are thermally coupled energy levels 4 F 9/2 The number of particles above;
ω 31 are thermally coupled energy levels 4 I 15/2 To a metastable state 6 H 13/2 Spontaneous emission rate of energy level transition;
ω 21 are thermally coupled energy levels 4 F 9/2 To a metastable state 6 H 13/2 Spontaneous emission rate of energy level transition;
g 31 are thermally coupled energy levels 4 I 15/2 To a metastable state 6 H 13/2 Energy level degeneracy of the energy level transition;
g 21 are thermally coupled energy levels 4 F 9/2 To a metastable state 6 H 13/2 Energy level degeneracy of the energy level transition;
ν 31 are thermally coupled energy levels 4 I 15/2 To a metastable state 6 H 13/2 The light emission frequency of the energy level transition;
ν 21 are thermally coupled energy levels 4 F 9/2 To a metastable state 6 H 13/2 The frequency of light emission of the energy level transition.
Thus, dy 3+ Ionic thermal coupling energy level 4 I 15/2 And 4 F 9/2 respectively to the ground state 6 H 15/2 Energy level and metastable state 6 H 13/2 Intensity (I) of blue light generated by energy level transition Blue light ＝I Blue light I +I Blue light II ) And yellow light intensity (I) Yellow light ) The ratio between can be expressed as:
wherein C 20 、C 21 、C 30 And C 31 Fitting is performed by experimental data for constants related to the emission light frequency, the degree of energy level degeneracy, and the emission frequency.
Wherein Δ E is 4 I 15/2 And 4 F 9/2 the energy difference between the two thermally coupled energy levels, k is the boltzmann constant and T is the absolute temperature.
Definition of temperature detection sensitivity according to equation (5) based on Dy 3+ The absolute sensitivity of the ion blue and yellow light intensity ratio for temperature measurement can be expressed as:
another object of the present invention is to protect a rare earth Dy 3+ A ratio-type temperature detection method of ion luminescence,
the method comprises the following specific steps:
s1, rare earth Dy 3+ Under the excitation of ultraviolet light or red light, the ion doped luminescent material is calculated to correspond to Dy at a certain temperature 3+ Ionic thermal coupling energy level 4 I 15/2 And 4 F 9/2 to the ground state 6 H 15/2 Blue down-or up-conversion of energy level transitions to luminescence intensity I Blue light ；
S2, calculating the temperature corresponding to Dy 3+ Ionic thermal coupling energy level 4 I 15/2 And 4 F 9/2 to a metastable state 6 H 13/2 Yellow upconversion luminescence intensity I of energy level transition Yellow light ；
S3, obtaining the fluorescence intensity ratio at the temperature
S4, changing rare earth Dy 3+ The temperature of the doped luminescent material is added, and the steps S1 to S3 are repeated to obtain the fluorescence intensity ratio
Temperature T;
s5, adopting a formula
Fitting the curve obtained in the step S4 to obtain the rare earth Dy 3+ The temperature detection is realized by the quantitative relation between the fluorescence intensity ratio of blue luminescence and yellow luminescence and the temperature.
Further, I Blue light ＝I Blue light I +I Blue light II Wherein, I Blue light I Is Dy 3+ Ionic thermal coupling energy level 4 I 15/2 To the ground state 6 H 15/2 Luminous intensity by energy level transition, I Blue light II Is Dy 3+ Ionic thermal coupling energy level 4 F 9/2 To the ground state 6 H 15/2 The intensity of light emission generated by energy level transition.
Further, I Yellow light ＝N 3 ω 31 g 31 hν 31 +N 2 ω 21 g 21 hν 21 。
Further, the ultraviolet light excitation wavelength is 352nm.
Further, the red light excitation wavelength is 698nm.
The rare earth Dy 3+ The technical characteristics of realizing high precision and high temperature sensing sensitivity temperature measurement by the fluorescence intensity ratio of blue luminescence and yellow luminescence are as follows:
a. by using rare earth Dy 3+ Ionic thermal coupling energy level 4 I 15/2 And 4 F 9/2 to the ground state 6 H 15/2 And metastable state 6 H 13/2 Blue and yellow down-or up-conversion luminescence intensity I of energy level transitions Blue colour And I Yellow colour Ratio of the luminous intensities of the two
Exhibits a specific quantitative relationship with the temperature T
b. The two luminescence in the ratio type temperature measurement method of the invention are from rare earth Dy 3+ Ionic thermal coupling energy level 4 I 15/2 And 4 F 9/2 respectively to the ground state 6 H 15/2 And metastable state 6 H 13/2 Transition of energy level, i.e. 4 I 15/2 / 4 F 9/2 → 6 H 15/2 And 4 I 15/2 / 4 F 9/2 → 6 H 13/2 . Due to the ground state 6 H 15/2 And metastable state 6 H 13/2 The difference between the energy levels is about 3000cm -1 Rare earth Dy 3+ The distance between the center positions of the ion blue and yellow luminous peaks is about 100nm, and the two luminous peaks do not overlap at all, so that the luminous intensity values of the blue light and the yellow light can be accurately calculated, and the problem of the luminescence caused by the overlapping of the two blue light luminous peaks is solvedThe light intensity measurement precision is low, so the measurement precision of the invention is high.
c. Due to thermal coupling of energy levels 4 I 15/2 And 4 F 9/2 follows the Boltzmann distribution, and thus thermally couples higher levels of energy levels at lower temperatures 4 I 15/2 Too low relative population of (2) results in its shifting to the ground state 4 I 15/2 The transition of energy level is weak and effective luminous intensity (i.e. I) cannot be obtained Blue light I ) Thus, conventionally based on Dy 3+ Method for measuring the ratio of two blue light intensities (i.e. I) Blue light I /I Blue light II ) Not applicable for lower temperature measurements. Dy based on which the present invention is based 3+ The blue and yellow luminescence of the ion can also obtain stronger luminescence intensity in a lower temperature range, and the ion can be suitable for low-temperature detection, so that the detection range of the temperature can be effectively expanded.
d. The invention is based on Dy 3+ The blue and yellow luminescence of ions can not only be excited by short wavelength such as ultraviolet light to obtain blue and yellow down-conversion luminescence, but also can be excited by easily obtained long wavelength such as red light to generate high-efficiency blue and yellow up-conversion luminescence as an excitation light source for temperature detection, so that the invention effectively expands the rare earth Dy-based luminescence 3+ The ratio type temperature measuring method has higher temperature detection sensitivity, does not reduce the temperature detection sensitivity, and even greatly improves the temperature detection sensitivity in some Dy doped fluorescent powder.
e. Dy based on which the present invention is based 3+ The specific theoretical relationship between the luminous intensity ratio of ion blue and yellow and the temperature is provided, and the method is suitable for all Dy 3+ The luminescent material is doped, so the invention has universality.
Drawings
FIG. 1 rare earth Dy 3+ The energy level structure and the light emission mechanism of the ions;
FIG. 2 shows Dy in example 1 of the present invention 3+ Doped CaWO 4 Excitation spectrum of phosphor at normal temperature (monitoring wavelength lambda) em =575 nm) (left panel a) and emission spectrum (excitation)Wavelength lambda ex =352nm (right panel a), and down-converted luminescence spectra (excitation wavelength λ) at different temperatures ex =352 nm) (fig. b);
FIG. 3 shows Dy in example 1 of the present invention 3+ Doped CaWO 4 Blue and yellow down-conversion luminescence intensity ratio (I) of the phosphor Blue light /I Yellow light ) Temperature (T) curve (graph a), and two blue down-conversion luminescence intensity ratios (I) Blue light I /I Blue light II ) Temperature (T) dependence (graph b);
FIG. 4 shows Dy in example 1 of the present invention 3+ Doped CaWO 4 The phosphor is based on the conversion luminescence intensity ratio (I) under blue and yellow colors respectively Blue light /I Yellow light ) And two blue down-conversion luminescence intensity ratios (I) Blue light I /I Blue light II ) Temperature sensitivity curve of (d);
FIG. 5 shows Dy of example 2 of the present invention 3+ Excitation spectrum of doped YAG phosphor at normal temperature (monitoring wavelength lambda) em =583 nm) (left panel a) and emission spectrum (excitation wavelength λ ex =352nm (right panel a), and down-converted luminescence spectra (excitation wavelength λ) at different temperatures ex =352 nm) (fig. b);
FIG. 6 shows Dy of example 2 of the present invention 3+ YAG phosphor doped blue and yellow down-conversion luminescence intensity ratio (I) Blue light /I Yellow light ) Temperature (T) dependence (graph a) and its temperature sensitivity curve (graph b);
FIG. 7 shows Dy in example 3 of the present invention 3+ Doping NaYF 4 Excitation spectrum of phosphor at normal temperature (monitoring wavelength lambda) em =575nm (right panel a) and emission spectrum (excitation wavelength λ ex =698 nm) (left side of fig. a), and upconversion luminescence spectra at different temperatures (excitation wavelength λ ex =698 nm) (fig. b);
FIG. 8 shows Dy in example 3 of the present invention 3+ Doping NaYF 4 The phosphor has a ratio of blue to yellow upconversion luminescence intensities (I) Blue light /I Yellow light ) The temperature (T) dependence (graph a) and its temperature sensitivity curve (graph b).
Detailed Description
The invention is described in more detail below with reference to specific examples, without limiting the scope of the invention. Unless otherwise specified, the experimental methods adopted by the invention are all conventional methods, and experimental equipment, materials, reagents and the like used in the experimental method can be obtained from commercial sources.
The invention uses rare earth Dy 3+ Doped CaWO 4 Fluorescent powder and Dy 3+ Doping with Y 3 Al 5 O 12 (YAG) phosphor and Dy 3+ Doping NaYF 4 The fluorescent powder is taken as 3 examples, ultraviolet light with 352nm and red light with 698nm are taken as excitation sources, and rare earth Dy is obtained 3+ Blue and yellow down-conversion luminescence and up-conversion luminescence of ions to realize rare earth Dy 3+ Quantitative relationship of ionic blue and yellow light intensity ratio to temperature.
Example 1
Rare earth Dy 3+ Doped CaWO 4 The phosphor converts luminescence at room temperature to Dy of inventive example 1 shown on the left side of FIG. 2a 3+ Doped CaWO 4 The fluorescence powder can be seen from the down-conversion excitation spectrum at normal temperature when the wavelength lambda is monitored em When yellow light emitting peak is 575nm, a plurality of Dy appear in the wave band range of 300-410 nm 3+ Wherein 352nm is the optimum excitation wavelength, corresponding to Dy 3+ Is 6 H 15/2 → 6 P 7/2 The transition is excited.
Dy of example 1 of the present invention shown from the right side of FIG. 2a 3+ Doped CaWO 4 The fluorescent powder can be seen from the down-conversion luminescence spectrum at normal temperature, and Dy is excited by 352nm ultraviolet light 3+ Doped CaWO 4 The fluorescent powder respectively emits blue light and yellow light which are converted to emit light within the wave band range of 420-650 nm and respectively correspond to Dy 3+ Of ions 4 I 15/2 → 6 H 15/2 ， 4 F 9/2 → 6 H 15/2 And 4 I 15/2 / 4 F 9/2 → 6 H 13/2 transition of, wherein 4 I 15/2 → 6 H 15/2 The transition is weak.
Dy of example 1 of the present invention shown in FIG. 2b 3+ Doped CaWO 4 The conversion luminescence spectrum of the fluorescent powder at different temperatures shows that Dy is improved along with the rise of the temperature 3+ The ion luminescence peak position is not obviously changed, but the luminescence intensity is changed. Corresponding to Dy 3+ Ion(s) in a substrate 4 F 9/2 → 6 H 15/2 And 4 I 15/2 / 4 F 9/2 → 6 H 13/2 blue light luminous intensity of transition I Blue light II And yellow luminous intensity I Yellow light All gradually decrease with increasing temperature, corresponding to 4 I 15/2 → 6 H 15/2 Blue light luminous intensity of transition I Blue light I Increasing slowly with increasing temperature.
S1, monitoring rare earth Dy by taking 352nm ultraviolet light as an excitation source 3+ Doped CaWO 4 The fluorescent powder corresponds to Dy in the range of 300-650K 3+ Ionic thermal coupling energy level 4 I 15/2 And 4 F 9/2 to the ground state 6 H 15/2 Blue down-conversion luminescence intensity I of energy level transition Blue light ；
S2, calculating the temperature range corresponding to Dy 3+ Ionic thermal coupling energy level 4 I 15/2 And 4 F 9/2 to a metastable state 6 H 13/2 Yellow upconversion luminescence intensity I of energy level transition Yellow light ；
S3, obtaining the fluorescence intensity ratio at the temperature
S4, changing rare earth Dy 3+ The temperature of the doped luminescent material is added, and the steps S1 to S3 are repeated to obtain the fluorescence intensity ratio
Temperature T;
s5, adopting a formula
Fitting the curve obtained in the step S4 to obtain the result of realizing the curve based onRare earth Dy 3+ The ratio of fluorescence intensity of blue and yellow luminescence was quantified as a function of temperature.
FIG. 3a shows Dy of example 1 of the present invention 3+ Doped CaWO 4 Dy of fluorescent powder 3+ Ion blue light emission intensity (I) Blue light ＝I Blue light I +I Blue light II ) Ratio of yellow light emission intensity (I) Blue light /I Yellow light ) And temperature (T), wherein the solid line is the fitting result of equation (7). Strength ratio (I) in the temperature range of 300-650K Blue light /I Yellow light ) And temperature (T) satisfies the good relationship shown in the formula (7), indicating that Dy 3+ The luminous intensity ratio of the blue light and the yellow light and the temperature show excellent temperature sensing characteristics in a wide temperature range.
Comparative example 1
For comparison, based on Dy 3+ Optical temperature sensing characteristics of two blue light intensity ratios, dy was also carried out by the inventors 3 + Doped CaWO 4 Dy-based phosphor 3+ The optical temperature sensing characteristics of two blue light intensity ratios were studied.
FIG. 3b shows Dy in example 1 of the present invention 3+ Doped CaWO 4 Dy in fluorescent powder 3+ Ion ratio of two blue light emission intensities (I) Blue light I /I Blue light II ) And temperature (T), wherein the solid line is the fitting result of equation (4).
Strength ratio (I) in the temperature range of 425-650K Blue light I /I Blue light II ) And temperature (T) satisfies formula (4), indicating Dy 3+ The ratio of the two blue luminous intensities of the ions to the temperature shows good temperature sensing characteristics in a higher temperature range. Whereas in the lower temperature region, there is a large deviation due to Dy at low temperature 3+ Ion(s) in a substrate 4 I 15/2 → 6 H 15/2 The transition is weak, and effective luminous intensity (I) cannot be obtained Blue light I ) And intensity ratio (I) Blue light I /I Blue light II )。
Calculation of Dy-based in example 1 according to equations (5) and (8), respectively 3+ Absolute sensitivity curve for temperature detection of ratio of blue light emission intensity to yellow light emission intensity and ratio of two blue light emission intensities
As can be seen from FIG. 4, dy was the basis for the entire experimental temperature range 3+ The temperature measurement technology of the luminous intensity ratio of the blue light and the yellow light has good temperature sensing sensitivity and has the maximum absolute sensitivity S when T =650K a ＝0.00243K -1 Compared with Dy-based 3+ Thermometry of two blue luminous intensity ratios (maximum sensitivity S at T = 600K) a ＝0.00125K -1 ) Improved by about 2 times, indicating that the Dy base of the invention 3+ Compared with the traditional Dy-based novel temperature measurement method based on the luminous intensity ratio of blue light and yellow light 3+ The temperature measurement method of the ratio of the two blue luminous intensities has higher temperature detection sensitivity.
Example 2
Rare earth Dy 3+ Doped YAG phosphor converts luminescence at room temperature to Dy from inventive example 2 shown on the left side of FIG. 5a 3+ The down-conversion excitation spectrum of the doped YAG fluorescent powder at normal temperature can be seen, and when the wavelength lambda is monitored em When yellow light emitting peak is 583nm, a plurality of Dy appear in the wave band range of 300-420 nm 3+ Wherein 352nm is still the optimum excitation wavelength, corresponding to Dy 3+ Is 6 H 15/2 → 6 P 7/2 The transition is excited. Dy of example 2 of the present invention shown from the right side of FIG. 5a 3+ The doped YAG fluorescent powder can be seen from the down-conversion luminescence spectrum at normal temperature, and Dy is excited by 352nm ultraviolet light 3+ The doped YAG fluorescent powder respectively emits blue within the wave band range of 440-630 nmColor and yellow down-conversion luminescence, corresponding to Dy 3+ Of ions 4 I 15/2 → 6 H 15/2 ， 4 F 9/2 → 6 H 15/2 And 4 I 15/2 / 4 F 9/2 → 6 H 13/2 transition, in which the energy level is thermally coupled 4 I 15/2 And 4 F 9/2 to the ground state 4 I 15/2 The two blue peaks of the energy level transition almost overlap.
Dy of example 2 of the present invention shown in FIG. 5b 3+ The conversion luminescence spectrum of the doped YAG fluorescent powder at different temperatures shows that Dy is increased along with the temperature 3+ The ion luminescence peak position is not obviously changed, but the luminescence intensity is changed. Corresponding to Dy 3+ Ion(s) in a substrate 4 F 9/2 → 6 H 15/2 And 4 I 15/2 / 4 F 9/2 → 6 H 13/2 blue light luminous intensity of transition I Blue light II And yellow luminous intensity I Yellow light All gradually decrease with increasing temperature, corresponding to 4 I 15/2 → 6 H 15/2 Blue light luminous intensity of transition I Blue light I Increasing slowly with increasing temperature.
Comparative example 2
Due to Dy 3+ Of ions 4 I 15/2 → 6 H 15/2 And 4 F 9/2 → 6 H 15/2 the two blue light emission peaks corresponding to the transitions are overlapped seriously, so that the two blue light emission intensities (I) cannot be calculated effectively Blue light I And I Blue light II ) Thus conventionally based on Dy 3+ Method for measuring the ratio of two blue light intensities of ions (i.e. I) Blue light I /I Blue light II ) Has great limitations.
The quantitative relationship between the intensity ratio of luminescence and temperature was calculated by the method of the present invention, and Dy of example 2 of the present invention is shown in FIG. 6a 3+ Dy doped with YAG fluorescent powder 3+ Ion ratio of blue to yellow luminous intensity (I) Blue light /I Yellow light ) And temperature (T), wherein the solid line is the formula(7) The fitting result of (1). Strength ratio (I) in the temperature range of 323-600K Blue light /I Yellow light ) And temperature (T) satisfies the good relationship shown in the formula (7), indicating that Dy 3+ The ratio of the luminous intensity of the blue light to the luminous intensity of the yellow light to the temperature shows excellent temperature sensing characteristics. FIG. 6b shows Dy-based calculated according to equation (8) 3+ The absolute sensitivity curve of the temperature detection of the luminous intensity ratio of the blue light and the yellow light can obtain the maximum absolute sensitivity S when T =426K a ＝0.0002K -1 。
Example 3
Rare earth Dy 3+ Doping NaYF 4 Phosphor up-converted to emit light at normal temperature, dy of inventive example 3 shown on right side of FIG. 7a 3+ Doping NaYF 4 The up-conversion excitation spectrum of the fluorescent powder at normal temperature can be seen, and when the wavelength lambda is monitored em When yellow light emitting peak is 575nm, a plurality of Dy appear in the wave band range of 650-850 nm 3+ Wherein 698nm is the optimum upconversion excitation wavelength corresponding to Dy 3+ Is/are as follows 6 H 15/2 → 6 P 7/2 Two-photon excitation of the transition. Dy of example 3 of the present invention shown on the left side of FIG. 7a 3+ Doping NaYF 4 The up-conversion luminescence spectrum of the fluorescent powder at normal temperature shows that Dy is excited by 698nm red light 3+ Doping NaYF 4 The fluorescent powder respectively emits blue and yellow up-conversion luminescence within the wave band range of 400-620 nm, which respectively corresponds to Dy 3+ Of ions 4 I 15/2 / 4 F 9/2 → 6 H 15/2 And 4 I 15/2 / 4 F 9/2 → 6 H 13/2 transition of thermal coupling energy level 4 I 15/2 And 4 F 9/2 to the ground state 4 I 15/2 The two blue peaks of the energy level transition overlap completely.
Dy of example 3 of the present invention shown in FIG. 7b 3+ Doping NaYF 4 The up-conversion luminescence spectra of the fluorescent powder at different temperatures show that Dy is increased along with the temperature 3+ The ion luminescence peak position is not obviously changed, but the luminescence intensity is changed. Corresponds to Dy 3+ Ion(s) 4 I 15/2 / 4 F 9/2 → 6 H 15/2 And 4 I 15/2 / 4 F 9/2 → 6 H 13/2 blue luminous intensity of transition I Blue light And yellow luminous intensity I Yellow light Both gradually decrease with increasing temperature.
Comparative example 3
Dy of inventive example 3 3+ Doping NaYF 4 Dy in fluorescent powder 3+ Ion(s) 4 I 15/2 → 6 H 15/2 And 4 F 9/2 → 6 H 15/2 two blue light emission peaks of the transition are basically and completely overlapped, and the intensity ratio of the two blue light emissions cannot be accurately obtained, so that the traditional optical temperature sensing characteristic based on the two blue light emission intensity ratios cannot be obtained.
FIG. 8a shows Dy of example 3 of the present invention 3+ Doping NaYF 4 Dy of fluorescent powder 3+ Ion ratio of blue to yellow luminous intensity (I) Blue light /I Yellow light ) And temperature (T), wherein the solid line is the fitting result of equation (7). Strength ratio (I) in the temperature range of 300-410K Blue light /I Yellow light ) And temperature (T) satisfies the good relationship shown in the formula (7), indicating that Dy 3+ The blue light and yellow light luminous intensity ratio and the temperature show excellent temperature sensing characteristics. FIG. 8b shows Dy-based calculated according to equation (8) 3+ The absolute sensitivity curve of the temperature detection of the luminous intensity ratio of the blue light and the yellow light can obtain the maximum absolute sensitivity S when T =300K a ＝0.001K -1 。
Dy cited above 3+ References to doped luminescent materials are as follows:
Dy 3+ doping with Y 4 Al 2 O 9 ：Z.Boruc,et al.,Optics Letters,2012,37,5214-5216；
Dy 3+ Doping BaYF 5 ：Z.Cao,et al.,Current Applied Physics,2014,14,1067-1071]；
Dy 3+ GdVO doping 4 ：Z.Antic,et al.,Advanced Materials,2016,28,7745-7752；
Dy 3+ Gd-doped 2 Ti 2 O 7 ：S.
et al.,Journal of Luminescence,2016,170,395-400；
Dy 3+ Doping with Y 2 SiO 5 ：L.M.Chepyga,et al.,Journal of Luminescence,2018,197,23-30；
Dy 3+ Doped CaWO 4 ：L.Li,et al.,Sensors and Actuators A:Physical,2020,304,111864。
The above description is only for the purpose of creating a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (5)
1. Rare earth-based Dy 3+ The ion-luminescent ratio-type temperature detection method is characterized in that ultraviolet or red light is used as an excitation source, and rare earth Dy 3+ Ionic thermal coupling energy level 4 I 15/2 And 4 F 9/2 respectively to the ground state 6 H 15/2 And metastable state 6 H 13/2 Carrying out energy level transition to generate blue and yellow down-conversion or up-conversion luminescence, and carrying out temperature detection according to the quantitative relation between the blue and yellow luminescence intensity ratio and the temperature;
wherein,
I blue light Blue luminous intensity, I Yellow light Yellow luminous intensity;
C 20 、C 21 、C 30 and C 31 For simplifying frequency and energy level of emitted lightThe parallelism and the constant related to the luminous frequency are obtained by fitting experimental data;
delta E is 4 I 15/2 And 4 F 9/2 an energy difference between the two thermally coupled energy stages;
k is Boltzmann constant;
t is the absolute temperature.
2. The method according to claim 1, characterized by the following specific steps:
s1, rare earth Dy 3+ Under the excitation of ultraviolet light or red light, the ion doped luminescent material is calculated to correspond to Dy at a certain temperature 3+ Ionic thermal coupling energy level 4 I 15/2 And 4 F 9/2 to the ground state 6 H 15/2 Blue down-or up-conversion of energy level transitions to luminescence intensity I Blue light ；
S2, calculating the temperature corresponding to Dy 3+ Ionic thermal coupling energy level 4 I 15/2 And 4 F 9/2 to a metastable state 6 H 13/2 Yellow upconversion luminescence intensity I of energy level transition Yellow light ；
S3, obtaining the fluorescence intensity ratio at the temperature
S4, changing rare earth Dy 3+ Doping the temperature of the luminescent material, and repeating the steps S1-S3 to obtain the fluorescence intensity ratio
A plot of absolute temperature T;
s5, adopting a formula
Fitting the curve obtained in the step S4 to obtain the rare earth Dy 3+ The temperature detection is realized by the quantitative relation between the fluorescence intensity ratio of blue and yellow luminescence and the temperature.
3. The method of claim 2, wherein I Yellow light ＝N 3 ω 31 g 31 hν 31 +N 2 ω 21 g 21 hν 21 ；
Wherein N is 3 Are thermally coupled energy levels 4 I 15/2 The number of particles above;
N 2 are thermally coupled energy levels 4 F 9/2 The number of particles above;
ω 31 are thermally coupled energy levels 4 I 15/2 To a metastable state 6 H 13/2 Spontaneous emission rate of energy level transition;
ω 21 are thermally coupled energy levels 4 F 9/2 To a metastable state 6 H 13/2 Spontaneous emission rate of energy level transition;
g 31 are thermally coupled energy levels 4 I 15/2 To a metastable state 6 H 13/2 Energy level degeneracy of the energy level transition;
g 21 are thermally coupled energy levels 4 F 9/2 To a metastable state 6 H 13/2 Energy level degeneracy of the energy level transition;
ν 31 are thermally coupled energy levels 4 I 15/2 To a metastable state 6 H 13/2 The light emission frequency of the energy level transition;
ν 21 are thermally coupled energy levels 4 F 9/2 To a metastable state 6 H 13/2 The frequency of light emission of the energy level transition.
4. The method of claim 2, wherein the ultraviolet light excitation wavelength is 352nm.
5. The method of claim 2, wherein the red light excitation wavelength is 698nm.
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