CN110330971B - High-sensitivity up-conversion temperature measurement material and preparation method and application thereof - Google Patents
High-sensitivity up-conversion temperature measurement material and preparation method and application thereof Download PDFInfo
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
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Abstract
The invention discloses a high-sensitivity up-conversion temperature measuring material, a preparation method and application thereof, and the structural formula of the material is MA2O4：xEr3+/yYb3+M is selected from Ca, Sr or Ba, A is selected from La or Lu, and x: y is 1-15: 20. the material uses 980nm laser as an excitation light source, emits emission peaks of thermal coupling energy level pairs at 540nm and 552nm respectively, and makes use of the particle number on the thermal coupling energy level of rare earth ions to follow the Boltzmann distribution rule, so that the particle number layout has a quantitative relation with the temperature, thereby realizing the measurement of the actual temperature. The method has the advantages of extremely small error, high sensitivity, effective realization of quick response and real-time monitoring on the slight change of the temperature, simple preparation, easy obtainment of raw materials, stability, reliability, low cost and the like, and is suitable for wide application and popularization.
Description
Technical Field
The invention relates to the technical field of temperature measurement of rare earth up-conversion luminescent materials, in particular to a high-sensitivity up-conversion temperature measurement material and a preparation method and application thereof.
Background
The temperature is one of important parameters for determining the state of a substance, and the measurement and control of the temperature play an important role in national defense, military, scientific experiments and industrial and agricultural production. In particular, high temperature measurement plays an extremely important role in the fields of aerospace, materials, energy, metallurgy and the like. At present, the most widely applied temperature measurement parts are thermocouples and thermal resistors, but the traditional methods are all contact temperature measurement methods, are easily influenced by the measurement environment, have poor dynamic property and real-time property, cause low measurement precision and large signal-to-noise ratio, and have great limitation in application.
The optical temperature measurement method has the advantages that light is used as a medium, so that the response is extremely quick, the optical temperature measurement method does not need to be in contact with a measured object, the incomparable advantages of the optical temperature measurement method become hot points of people's attention and research, the dependence of the luminous intensity of the luminous material on temperature can also be used for temperature measurement, the optical temperature measurement method is generally divided into a fluorescence intensity type temperature sensor and a fluorescence intensity ratio type temperature sensor, compared with the fluorescence intensity type temperature sensor, the pump light source of the fluorescence intensity type temperature sensor is easy to bring errors when the pump light source disturbs the fluorescent material in the excitation process, and the fluorescence intensity ratio type temperature sensor is more accurate. Especially, in the up-conversion rare earth material, the particle number of the rare earth ion energy level accords with the Boltzmann distribution, when the temperature changes, the particle book layout on each energy level changes, the response of different energy levels to the temperature change is different, and therefore the fluorescence intensity change corresponding to each energy level is also different. The fluorescence intensities of the rare earth doped up-conversion luminescent material at different temperatures are monitored by selecting a proper thermal coupling energy level pair, and the fluorescence intensity ratio is calculated to indirectly know the temperature, which is the basic process of temperature measurement of the rare earth doped up-conversion luminescent material. Therefore, the rare earth doped up-conversion material has the advantages of non-contact temperature measurement, rapid light-temperature response, strong environmental electromagnetic interference resistance, high tolerance on light source power fluctuation and high spatial resolution of temperature measurement, and has a great application prospect in the field of optical temperature sensing.
The invention patent CN201811240605.2 discloses a fluorescence color-changing optical temperature measuring material with a structural general formula of Ca3-m-nSrmZnLi(VO4)3:Eun 3+，Eu3+For activating ions, the material is effectively excited by ultraviolet light, and the [ VO ] of matrix4]3-Group and activated ion Eu3+As a dual luminescence center, emits respective characteristic spectra simultaneously. Because the thermal quenching properties of the two luminescent centers are different, the color coordinates (x, y) corresponding to the luminescent colors of the material meet the linear equation track along with the change of temperature, and based on the linear equation track, the temperature can be roughly and qualitatively calibrated by utilizing the fluorescent discoloration under the excitation of ultraviolet light, but the method utilizes the fluorescent discoloration for temperature measurement, has large error and low precision, and a fitting formula does not have a basic physical basis for support; the invention patent CN201710331934.7 discloses an optical temperature measuring material with high sensitivity and a preparation method thereof, and the chemical composition formula is (La)1-xPrx)2MgTiO6Wherein, the doped ion is Pr3+X is a doping ion Pr3+Relative rare earth metal ion La3+Is occupied by mole percentageThe value range of the coefficient is more than or equal to 0.0025 and less than or equal to 0.05, but the optical temperature measuring material prepared by the method has low luminous intensity, poor sensitivity and large error, and can not effectively and accurately realize quick response and real-time monitoring on temperature. Therefore, it is important to develop a new thermometric material with high sensitivity.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a high-sensitivity up-conversion temperature measuring material and a preparation method thereof, and solves the problems of large error and low luminous intensity of the existing optical temperature measuring material.
The invention also provides the application of the high-sensitivity up-conversion temperature measuring material, the material is very accurate in temperature measurement, the error is extremely small, and quick response and real-time monitoring on slight temperature change are effectively realized.
In order to solve the technical problems, the invention adopts the following technical scheme: a high-sensitivity up-conversion temperature measuring material with a general formula of MA2O4：xEr3+/yYb3+M is selected from Ca, Sr or Ba, A is selected from La, Lu, x: y is 20: 1-15; wherein, Er3+Is an activator, Yb3+Is a sensitizer.
Preferably, the value of x is 0.01-0.15, and the value of y is 0.20.
Preferably, a is introduced in the form of a simple substance a or a compound containing a ions, M is introduced in the form of a simple substance M or a compound containing M ions, and Er and Yb are introduced in the form of compounds containing Er ions and Yb ions, respectively.
Preferably, the compound is an oxide, nitrate or carbonate.
The invention also provides a preparation method of the high-sensitivity up-conversion temperature measuring material, which comprises the following steps:
1) taking corresponding raw materials according to the stoichiometric ratio of each substance in the general formula of the structural formula, and uniformly grinding the raw materials to obtain a mixture;
2) and (2) calcining the mixture obtained in the step 1) in a high-temperature furnace, naturally cooling and grinding after the reaction is finished, and obtaining powder with the body color from white to pink, namely the high-sensitivity up-conversion temperature measuring material.
Preferably, the calcining temperature is 1300-1500 ℃, and the calcining time is 4-8 h.
The invention also provides application of the high-sensitivity up-conversion temperature measuring material, the material is placed in an environment to be measured, 980nm near infrared continuous excitation is adopted as a laser light source, the fluorescence intensity ratio emitted by thermal coupling energy levels at 540nm and 552nm is calculated, and then the temperature of the environment to be measured is obtained according to the quantitative relation between the fluorescence intensity ratio emitted by the thermal coupling energy levels and the temperature of the environment to be measured.
Preferably, the power of the excitation light source is 0-3W, and the focal spot diameter is less than or equal to 5 mm. The up-conversion fluorescent material has good luminous intensity, can obtain strong luminescence only by milliwatt laser power, is beneficial to energy conservation, effectively reduces the heat effect brought by an excitation light source, and is more accurate in temperature measurement.
Preferably, the quantitative relationship between the Fluorescence Intensity (FIR) ratio emitted by the thermal coupling energy level and the environmental temperature (T) to be measured is obtained by fitting the fluorescence intensity ratios emitted by the thermal coupling energy levels at 540nm and 552nm based on the principle of least squares, as shown in formula (2):
preferably, the interval of the environment to be measured T is 318-538K.
For Er3+To say, energy level2H11/2Sum energy level4S3/2The energy band difference is 750-850 cm-1So that these two energy levels meet the requirements of a thermally coupled energy level pair; upper thermal coupling energy level during temperature change2H11/2Can be thermally coupled down to an energy level4S3/2The electron filling is carried out, when the temperature is stable, so that new thermal coupling balance is achieved and the Boltzmann distribution is followed; near 980nmUnder the excitation of infrared laser, the luminous intensity of corresponding energy level also changes with the temperature change, the invention adopts fluorescence intensity technology (FIR), can well convert the temperature quantity into corresponding numerical value, thus obtain the measured temperature. The invention is used for actual temperature measurement, and is expected to redefine the temperature measurement accuracy.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the upconversion fluorescent material prepared by the invention, 980nm laser is used as an excitation light source, emission peaks of thermal coupling energy levels are respectively emitted at 540nm and 552nm, and a determined functional relation between the integral intensity ratio of the thermal coupling energy levels and the temperature can be obtained through a light-emitting waveband of the thermal coupling energy levels in a rare earth ion upconversion spectrum, so that the temperature to be measured is converted into a visible numerical value, and the purpose of measuring the temperature is achieved. The invention can realize non-contact measurement of temperature under complex environment and extreme conditions, reduces the dependence on the measurement environment, is basically not influenced by the power fluctuation of pump laser and external factors such as water vapor, dust and the like in the light path transmission process, and can obviously improve the measurement precision and the signal-to-noise ratio.
2. The method utilizes the particle number on the thermal coupling energy level in the microstructure to follow the Boltzmann distribution rule, and fits the fluorescence intensity ratio emitted by the thermal coupling energy level at 540nm and 552nm based on the least square method principle to obtain the quantitative relation between the Fluorescence Intensity (FIR) ratio emitted by the thermal coupling energy level and the environmental temperature (T) to be measured.
3. The optical temperature measuring material is synthesized by a high-temperature solid-phase method, the preparation and operation processes are safe, the reaction conditions are easy to control, and the introduction of special atmosphere or harsh environments such as high pressure and the like is not needed. With MA2O4(M ═ Ca, Sr, Ba; A ═ La, Lu) is the substrate, its physical and chemical properties are stable, can exist stably in the air, the up-conversion fluorescent material prepared by said substrate has good luminous intensity, only uses milliwatt laser power can obtain strong luminescence, it is beneficial to energy-saving and can effectively reduce the heat effect brought by exciting light sourceMore accurate in temperature measurement, further less error. The invention has the advantages of easily obtained raw materials, stability, reliability and low cost, and is suitable for wide application and popularization.
4. The fitting degree of the functional relation presented by the fluorescence intensity ratio and the temperature of the up-conversion fluorescent material in the temperature range of 318K-538K is very high, which indicates that the material is very accurate in temperature measurement and has very small error; while the defined sensitivity can reach 0.22% K at 498K-1The response sensitivity to temperature is obviously superior to that of the conventional optical method at present; therefore, the invention effectively realizes the quick response and real-time monitoring of the slight change of the temperature, and has good application prospect.
Drawings
FIG. 1 shows the up-conversion phosphor SrLu prepared in example 12O4:Er3+/Yb3+X-ray diffraction patterns of (a); from top to bottom sequentially is SrLu2O4:5％Er3+/20％Yb3+Measured XRD patterns and SrLu of samples2O4A standard card XRD pattern;
FIG. 2 shows the up-conversion phosphor SrLu prepared in example 12O4:5％Er3+/20％Yb3+Fluorescence emission spectra excited at different temperatures;
FIG. 3 shows the up-conversion phosphor SrLu prepared in example 12O4:5％Er3+/20％Yb3+The FIR curve relation of the fluorescence intensity ratio and the temperature;
FIG. 4 shows the up-conversion phosphor SrLu prepared in example 12O4:5％Er3+/20％Yb3+Sensitivity curves at different temperatures.
Detailed Description
The present invention will be described in further detail with reference to examples. The reagents used in the examples were either high purity (4N) or guaranteed grade, and are not specifically described as being commercially available.
Preparation method of high-sensitivity up-conversion temperature measuring material
Example 1
1) Weighing 1.4763g of solid powder strontium carbonate, 3.9845g of solid powder lutetium oxide, 0.3941g of solid powder ytterbium oxide and 0.0956g of solid powder erbium oxide, putting the raw materials into an agate mortar, fully grinding and mixing for 1h to obtain a mixture, pouring the mixture into a corundum crucible, and covering;
2) placing the corundum crucible in the step 1) in a high-temperature furnace, heating to 1300 ℃, heating at constant temperature for 6h, naturally cooling to room temperature after the reaction is finished, then placing the fired sample in an agate mortar, and grinding into powder to obtain the up-conversion fluorescent powder SrLu2O4：5％Er3+/20％Yb3+。
The upconversion phosphor SrLu prepared in the example2O4：5％Er3+/20％Yb3+The analysis was carried out by X-ray diffraction technique, and the results are shown in FIG. 1.
As can be seen from FIG. 1, SrLu2O4:5％Er3+/20％Yb3+Measurement of XRD and SrLu of sample2O4The standard card XRD can completely correspond to each other, and no impurity peak exists, which indicates that the synthesized sample is successful and pure in components, and the sample synthesized by the method is pure phase.
Example 2
1) Weighing 1.0009g of solid powder calcium carbonate, 3.9845g of solid powder lutetium oxide, 0.3941g of solid powder ytterbium oxide and 0.0956g of solid powder erbium oxide, putting the raw materials into an agate mortar, fully grinding and mixing for 1h to obtain a mixture, pouring the mixture into a corundum crucible, and covering the corundum crucible;
2) placing the corundum crucible in the step 1) in a high-temperature furnace, heating to 1300 ℃, heating at constant temperature for 6h, naturally cooling to room temperature after the reaction is finished, then placing the fired sample in an agate mortar, and grinding into powder to obtain the up-conversion fluorescent powder CaLu2O4:5％Er3+/20％Yb3+。
Example 3
1) Weighing 1.9734g of solid powder barium carbonate, 3.9845g of solid powder lutetium oxide, 0.3941g of solid powder ytterbium oxide and 0.0956g of solid powder erbium oxide, putting the raw materials into an agate mortar, fully grinding and mixing for 1h to obtain a mixture, pouring the mixture into a corundum crucible, and covering;
2) placing the corundum crucible in the step 1) in a high-temperature furnace, heating to 1300 ℃, heating at constant temperature for 6h, naturally cooling to room temperature after the reaction is finished, then placing the fired sample in an agate mortar, and grinding into powder to obtain the up-conversion fluorescent powder BaLu2O4:5％Er3+/20％Yb3+。
Example 4
1) Weighing 1.9734g of solid powder barium carbonate, 3.2581g of solid powder lanthanum oxide, 0.3941g of solid powder ytterbium oxide and 0.0191g of solid powder erbium oxide, putting the raw materials into an agate mortar, fully grinding and mixing for 1h to obtain a mixture, pouring the mixture into a corundum crucible, and covering;
2) placing the corundum crucible in the step 1) in a high-temperature furnace, heating to 1400 ℃, heating at constant temperature for 5h, naturally cooling to room temperature after the reaction is finished, then placing the fired sample in an agate mortar, and grinding into powder to obtain the up-conversion fluorescent powder BaLa2O4:1％Er3+/20％Yb3+。
Example 5
1) Weighing 1.0009g of solid powder calcium carbonate, 3.2581g of solid powder lanthanum oxide, 0.3941g of solid powder ytterbium oxide and 0.0191g of solid powder erbium oxide, putting the raw materials into an agate mortar, fully grinding and mixing for 1 hour to obtain a mixture, pouring the mixture into a corundum crucible, and covering;
2) placing the corundum crucible in the step 1) in a high-temperature furnace, heating to 1400 ℃, heating at constant temperature for 5h, naturally cooling to room temperature after the reaction is finished, then placing the fired sample in an agate mortar, and grinding into powder to obtain the up-conversion fluorescent powder CaLa2O4:1％Er3+/20％Yb3+。
Example 6
1) Weighing 1.4763g of solid powder strontium carbonate, 3.2581g of solid powder lanthanum oxide, 0.3941g of solid powder ytterbium oxide and 0.0191g of solid powder erbium oxide, putting the raw materials into an agate mortar, fully grinding and mixing for 1h to obtain a mixture, pouring the mixture into a corundum crucible, and covering;
2) placing the corundum crucible in the step 1) in a high-temperature furnace, heating to 1400 ℃, heating at constant temperature for 5h, naturally cooling to room temperature after the reaction is finished, then placing the fired sample in an agate mortar, and grinding into powder to obtain the up-conversion fluorescent powder SrLa2O4:1％Er3+/20％Yb3+。
Second, application of high-sensitivity up-conversion temperature measuring material
The spectrum of the up-conversion fluorescent powder obtained by the invention can obviously distinguish Er3+Of ions2H11/2And4S3/2the energy state returns to the fluorescence peak emitted by the ground state, ensuring that the two fluorescence peaks do not overlap to a large extent.2H11/2And4S3/2the central positions of the fluorescence peaks emitted by the energy states are respectively positioned at 540nm and 552nm, and Er is obtained under 980nm laser pumping3+The ion ground state energy level absorbs the exciting light and then transits to2H11/2And4S3/2on the energy level, in the thermal equilibrium state,2H11/2and4S3/2the particle distribution on the energy level meets the Boltzmann statistical distribution rule, and the distribution of the particle number has a determined corresponding relation with the temperature. Er3+Ion(s)2H11/2And4S3/2the quantitative relationship between the fluorescence intensity ratio corresponding to the energy level and the temperature is as follows (1):
in the formula IHAnd ISRespectively energy level2H11/2Sum energy level4S3/2(ii) spectrally integrated intensity; n is a radical ofHAnd NSIs the number of particles at the corresponding energy level; g, A, σ, and ω are the degree of degeneracy, radiative relaxation rate, emission interface and angular frequency, respectively, Δ E is the energy band difference between thermally coupled energy level pairs, KBBoltzmann constant and T is the temperature to be measured, C is a complex exponential constant.
The up-conversion phosphor SrLu prepared in example 12O4：5％Er3+/20％Yb3+The sample is excited under 980nm laser with the laser power of 0-3W and the focal spot diameter less than or equal to 5mm, and then the sample is heated to 318K/338K/ 358K/ 378K/ 398K/ 418K/ 438K/ 458K/ 478K/ 498K/518K and 538K respectively to obtain the temperature-variable spectral data of the sample, as shown in FIG. 2.
As can be seen from FIG. 2, Er gradually increases from 318K to 538K3+The emission intensity of the thermally coupled energy level pair of the ion changes with the temperature, the temperature rises, and the upper thermally coupled energy level2H11/2Has an increased emission intensity, a lower thermal coupling energy level4S3/2The emission intensity of (2) is decreased, and a reverse change phenomenon is exhibited.
Obtaining the fluorescence intensity ratio by using the fluorescence intensity ratio technology according to the obtained temperature-variable spectrum data, fitting the fluorescence intensity ratio with the tested temperature, calculating a correlation coefficient, verifying the conformity of the fitting curve and the experimental result, and determining a quantitative relation between the fluorescence intensity ratio and the temperature, wherein the function relation is as shown in fig. 3:
in the figure, the fitting curve of the FIR can be well fitted with the experimental points, the fitting degree reaches more than 99%, which shows that the fitting degree of the function is very high, which shows that the invention has very accurate measurement on temperature and very small error, and shows that the upconversion fluorescent powder has excellent temperature measurement performance.
The up-conversion phosphor SrLu prepared in example 12O4：5％Er3+/20％Yb3+Placing the sample in an environment to be tested, and placing SrLu2O4：5％Er3+/20％Yb3+Exciting under 980nm laser (the laser power is 0-3W, and the focal spot diameter is less than or equal to 5mm), and substituting the generated thermal coupling energy level to the fluorescence intensity ratio into the function to obtain the temperature of the environment to be measured.
Third, sensitivity
The fluorescence intensity ratio formula is derived, and the relation formula of the temperature measurement sensitivity is obtained and is shown as the following formula (3):
bringing the variable temperature spectral data obtained in the figure 2 into formula (3) to obtain the up-conversion fluorescent powder SrLu2O4：5％Er3+/20％Yb3 +The temperature measurement sensitivity of (2) is shown in fig. 4 as a function of temperature.
As can be seen from the graph, the maximum sensitivity value is 0.22% K at around 500K in the temperature range of 318K to 538K-1The sensitivity level is better than the response sensitivity of the conventional optical method to the temperature at present. Compared with the conventional optical method, the upconversion fluorescent powder prepared by the invention has good sensitivity and temperature resolution.
The above description is only exemplary of the present invention and should not be taken as limiting, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The application of the high-sensitivity up-conversion temperature measuring material is characterized by comprising the high-sensitivity up-conversion temperature measuring material with the structural formula of MA2O4：xEr3+/yYb3+M is selected from Ca, Sr or Ba, A is selected from La or Lu, and x: y is 1-15: 20;
placing the material in an environment to be measured, adopting a laser light source for 980nm near infrared continuous excitation, calculating the fluorescence intensity ratio of the spectrums emitted by the thermal coupling energy levels at 540nm and 552nm, and obtaining the temperature of the environment to be measured according to the quantitative relation between the fluorescence intensity ratio emitted by the thermal coupling energy levels and the temperature of the environment to be measured;
the quantitative relation between the Fluorescence Intensity (FIR) ratio emitted by the thermal coupling energy level and the environment temperature (T) to be measured is obtained by fitting the fluorescence intensity ratios emitted by the thermal coupling energy levels at 540nm and 552nm based on the principle of least squares, and the formula (2) is as follows:
2. the application of the high-sensitivity up-conversion temperature measuring material according to claim 1, wherein x is 0.01-0.15, and y is 0.20.
3. The use of the high-sensitivity up-conversion temperature measuring material according to claim 1, wherein A is introduced in the form of a simple substance A or a compound containing A ions, M is introduced in the form of a simple substance M or a compound containing M ions, and Er and Yb are introduced in the form of a compound containing Er ions and Yb ions, respectively.
4. The use of the high-sensitivity up-conversion thermometric material of claim 3, wherein the compound is an oxide, a nitrate or a carbonate.
5. The application of the high-sensitivity up-conversion temperature measuring material according to claim 1, wherein the power of the laser light source is 0-3W, and the focal spot diameter is less than or equal to 5 mm.
6. The application of the high-sensitivity up-conversion temperature measuring material according to claim 1, wherein the range of the environment T to be measured is 318-538K.
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