CN111073643A - Temperature probe material with europium and manganese elements doped together and preparation method thereof - Google Patents
Temperature probe material with europium and manganese elements doped together and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of temperature sensing, in particular to a temperature sensing material with europium and manganese elements doped together and a preparation method thereof. The temperature measuring material has an atomic ratio composition represented by general formula (1): (Na)1‑xLix)(La1‑y‑z‑mGdyYz)MgW1‑nO6:Eum 3+,Mnn 4+(1) (ii) a Wherein x, y and z satisfy the following conditions: x is more than or equal to 0 and less than or equal to 0.5, y is more than or equal to 0 and less than or equal to 0.3, and z is more than or equal to 0 and less than or equal to 0.3; m and n satisfy the following conditions: 0<m≤0.1，0<n is less than or equal to 0.02. The temperature measuring material disclosed by the invention is simple and safe in preparation conditions. The prepared temperature measuring material can accurately calibrate the temperature by utilizing the luminous intensity ratio of the double luminous centers, has a wide temperature measuring range and high signal detection discrimination.
Description
Technical Field
The invention relates to the technical field of temperature sensing, in particular to a temperature sensing material with europium and manganese elements doped together and a preparation method thereof.
Background
With the rapid development and progress of 5G and Internet of things technologies, various sensors are applied in a large quantity, and higher requirements are provided for real-time online detection of temperature. In this context, temperature measurement represented by an optical temperature sensing technique is becoming a hot spot of research.
At a certain temperature, some optical characteristics of the fluorescent material change along with the change of the temperature, so that the change of the optical properties of the fluorescent material can be used for measuring the temperature. The conventional fluorescence temperature measurement mode is to select single rare earth luminescent ion as an activator to be doped into a main body matrix by using a fluorescence intensity ratio method, and then select two energy levels with relatively close luminescent ion positions as a thermal coupling pair to realize temperature measurement. In order to realize the condition of thermal coupling temperature measurement of the single rare earth luminescent ion, the energy level of the thermal coupling must be within a small range, and if the energy level is too large, the decoupling phenomenon occurs. If the energy level is too small, the temperature measurement sensitivity is too low. Therefore, the single rare earth luminescent ion thermal coupling temperature measurement mode cannot realize simultaneous optimization and improvement of temperature measurement sensitivity and signal discrimination.
For this reason, it is of great practical importance to develop a new high-sensitivity temperature measurement material based on a luminescent material.
Disclosure of Invention
The invention aims to solve the technical problem of providing an optical temperature measuring material based on common doping of elements europium and manganese and a preparation method thereof, the temperature measuring material overcomes the defects of the traditional single rare earth luminescent ion thermal coupling temperature measuring material, the temperature measuring material has high sensitivity due to the dual-luminescence characteristic formed by common doping of the elements europium and manganese, the preparation method is simple and safe, the temperature is accurately measured by utilizing the fluorescence intensity ratio of the dual-luminescence center, and the optical temperature measuring material has the characteristics of wide temperature measuring range and high signal monitoring discrimination.
Specifically, the technical scheme of the invention is as follows:
the invention discloses a temperature measuring material based on co-doping of europium and manganese elements, which has the atomic ratio composition represented by the following general formula (1):
(Na1-xLix)(La1-y-z-mGdyYz)MgW1-nO6:Eum 3+,Mnn 4+(1)
wherein x, y and z satisfy the following conditions: x is more than or equal to 0 and less than or equal to 0.5, y is more than or equal to 0 and less than or equal to 0.3, and z is more than or equal to 0 and less than or equal to 0.3; m and n satisfy the following conditions: m is more than 0 and less than or equal to 0.1, and n is more than 0 and less than or equal to 0.02.
It should be understood that the specific atomic ratio composition of the thermometric material of the present invention is not limited to the above-described composition, and any suitable composition is within the scope of the present patent application.
Preferably, the thermometric material can be used as a material of a temperature probe.
Further, the thermometric material has an atomic ratio composition represented by the following general formula (2):
(Na0.9Li0.1)(La0.75Gd0.1Y0.1)MgW0.997O6:Eu0.05 3+,Mn0.003 4+(2)
wherein x is 0.1, y is 0.1, z is 0.1, m is 0.05, and n is 0.003.
Further, the thermometric material has an atomic ratio composition represented by the following general formula (3):
(Na0.5Li0.5)(La0.35Gd0.3Y0.3)MgW0.99O6:Eu0.05 3+,Mn0.01 4+(3)
wherein x is 0.5, y is 0.3, z is 0.3, m is 0.05, and n is 0.01.
Further, the thermometric material has an atomic ratio composition represented by the following general formula (4):
(Na1.0Li0.0)(La0.95Gd0.0Y0.0)MgW0.995O6:Eu0.05 3+,Mn0.005 4+(4)
wherein x is 0.0, y is 0.0, z is 0.0, m is 0.05, and n is 0.005.
Furthermore, the temperature measuring material is in the form of powder, a film or ceramic.
It should be understood that the form of the thermometric material of the present invention is not limited to the above-described form, and any suitable form is within the scope of the present patent application.
The second aspect of the invention discloses a method for preparing the element europium and manganese codoped temperature measuring material, which comprises the following steps:
respectively weighing compounds containing elements Na, Li, La, Gd, Y, Eu, Mg, W and Mn according to the atomic ratio, grinding the compounds, calcining, cooling to room temperature, and grinding to obtain a temperature measuring material; or the like, or, alternatively,
respectively weighing compounds containing elements Na, Li, La, Gd, Y, Eu, Mg, W and Mn according to the atomic ratio, dissolving the compounds in water to obtain a mixed solution, adding organic acid into the mixed solution, drying to form gel, and sintering the gel to obtain the temperature measuring material.
Further, the compound is carbonate, nitrate, oxide or hydroxide corresponding to the above elements. Further, the compound is a nitrate containing the elements Na, Li, La, Gd, Y, Eu, Mg, W and Mn.
Further, the organic acid is citric acid.
Further, sintering is carried out in two stages, the first stage: sintering for 1-3h at the temperature of 400-; the second stage is as follows: sintering for 2-10h under the conditions of 1000-1200 ℃.
The third aspect of the invention discloses a method for obtaining the temperature measurement value of the environment to be measured by the temperature measurement material, which comprises the following steps:
step one, testing emission spectra of temperature measuring materials at different temperatures, and establishing a standard working curve of integral luminous intensity ratio of trivalent europium Eu (III) emission peak and tetravalent manganese Mn (IV) emission peak along with temperature change;
placing the temperature measuring material in a temperature environment to be measured, and measuring the emission spectrum of the temperature measuring material to further obtain the integral luminous intensity ratio of the emission peak of trivalent europium Eu (III) and the emission peak of tetravalent manganese Mn (IV);
and step three, obtaining the temperature measurement value of the environment to be measured through a standard working curve according to the integral luminous intensity ratio of the environment to be measured.
Further, the integrated luminous intensity ratio and the absolute temperature satisfy the following exponential equation:
FIR＝IEu3+/IMn4+＝A×exp(B/T)+C；
wherein FIR is the ratio of integrated luminous intensity, T is absolute temperature, IEu3+And IMn4+The integrated luminescence intensities of the emission peaks of trivalent europium Eu (III) and tetravalent manganese Mn (IV), A, B, C are constants respectively.
On the basis of the common general knowledge in the field, the above-mentioned preferred conditions can be combined arbitrarily without departing from the concept and the protection scope of the invention.
Compared with the prior art, the invention has the following remarkable advantages and effects:
the preparation method prepares the temperature measuring material under normal pressure and air atmosphere, does not need reducing atmosphere synthesis, and has simple and safe preparation conditions. Under the effective excitation of ultraviolet light, trivalent europium Eu (III) and tetravalent manganese Mn (IV) are used as double luminescence centers to simultaneously emit respective characteristic spectrums, the integral luminescence intensity ratio of the trivalent europium Eu (III) and the tetravalent manganese Mn (IV) is regularly changed along with the temperature, a standard working curve can be used for fitting, and the characteristic emission peaks with far distance of the two wavelengths of the trivalent europium Eu (III) and the tetravalent manganese Mn (IV) are detected, so that high signal discrimination is obtained, and the mutual interference of detection signals is avoided. The temperature can be accurately calibrated by utilizing the luminous intensity ratio of the double luminous centers, and the prepared temperature measuring material has wide temperature measuring range and high signal detection discrimination.
Drawings
FIG. 1 is an X-ray powder diffraction pattern of a temperature measuring material disclosed in examples 1, 2 and 7 of the present invention;
FIG. 2 is a spectrum of an emission spectrum of the thermometric material of example 1 of the present invention under the excitation of an ultraviolet light source;
FIG. 3 is a graph showing the variation of the luminescence intensity ratio with temperature and the corresponding fitting curve of the thermometric material in example 1 of the present invention.
Detailed Description
The technical solutions of the present invention are described in detail below with reference to the drawings and the embodiments, but the present invention is not limited to the scope of the embodiments.
The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions. The reagents and starting materials used in the present invention are commercially available.
Example 1
The embodiment discloses a preparation method of a temperature measuring material, which comprises the following specific atomic ratio components: (Na)0.9Li0.1)(La0.75Gd0.1Y0.1)MgW0.997O6:Eu0.05 3+,Mn0.003 4+。
The preparation method comprises the following steps:
(1) accurately weighing carbonate containing Na, Li, Mg, W and Mn and oxide containing La, Gd, Y and Eu according to specific atomic ratio;
(2) the compound raw materials are fully ground and mixed, then are calcined for 2 to 10 hours at the temperature of between 1000 and 1200 ℃, and are cooled to room temperature and ground to obtain the temperature measuring material.
The X-ray powder diffraction pattern of the thermometric material disclosed in example 1 is included in figure 1 and compared to a standard card shows that the pure phase is synthesized.
FIG. 2 is a spectrum of an emission spectrum of the thermometric material disclosed in example 1 under the excitation of an ultraviolet light source, and it can be clearly seen from the graph that trivalent europium Eu (III) and tetravalent manganese Mn (IV) as dual luminescence centers can simultaneously and respectively emit respective characteristic emission peaks under the effective excitation of ultraviolet light.
FIG. 3 is a graph of the relationship between the ratio of the luminous intensity of the thermometric material and the temperature and the corresponding fitting curve as disclosed in example 1. The ratio FIR of the luminous intensity of the double luminous centers to the absolute temperature T meets the following exponential equation,
FIR＝IEu3+/IMn4+＝A*exp(B/T)+C，
wherein, IEu3+And IMn4+The integrated luminescence intensity respectively represents the characteristic emission peaks of trivalent europium Eu (III) and tetravalent manganese Mn (IV), A, B, C is a constant, and T is absolute temperature.
By detecting the emission spectra of the temperature measuring material at different temperatures, experimental data points of the fluorescence intensity ratio FIR and the absolute temperature T of the double luminescence centers are obtained, and the standard working curve equation of the temperature measuring material in the embodiment is obtained by fitting an exponential equation as follows:
FIR＝IEu3+/IMn4+＝66.04×exp(-2702/T)+0.055。
example 2
Embodiment 2 discloses a method for preparing a temperature measuring material based on element europium and manganese codoping, which is the only difference from the preparation method of embodiment 1, the weighing amounts of the carbonate containing elements Na, Li, Mg, W and Mn and the oxide containing elements La, Gd, Y and Eu in the step (1) are different, and the specific atomic ratio composition of the finally prepared temperature measuring material is as follows: (Na)0.5Li0.5)(La0.35Gd0.3Y0.3)MgW0.99O6:Eu0.05 3+,Mn0.01 4。
Example 3
Embodiment 3 discloses a method for preparing a temperature measuring material based on element europium and manganese codoping, which is the only difference from the preparation method of embodiment 1, the weighing amounts of the carbonate containing elements Na, Li, Mg, W and Mn and the oxide containing elements La, Gd, Y and Eu in the step (1) are different, and the specific atomic ratio composition of the finally prepared temperature measuring material is as follows: (Na)0.9Li0.1)(La0.75Gd0.1Y0.1)MgW0.995O6:Eu0.05 3+,Mn0.005 4+。
Example 4
Example 5
Embodiment 5 discloses a method for preparing a temperature measuring material based on element europium and manganese codoping, which is the only difference from the preparation method of embodiment 1, the weighing amounts of the carbonate containing elements Na, Li, Mg, W and Mn and the oxide containing elements La, Gd, Y and Eu in the step (1) are different, and the specific atomic ratio composition of the finally prepared temperature measuring material is as follows: na (Na)0.9Li0.1)(La0.79Gd0.1Y0.1)MgW0.99O6:Eu0.01 3+,Mn0.01 4+。
Example 6
Embodiment 6 discloses a method for preparing a temperature measuring material based on element europium and manganese codoping, which is the only difference from the preparation method of embodiment 1, the weighing amounts of the carbonate containing elements Na, Li, Mg, W and Mn and the oxide containing elements La, Gd, Y and Eu in the step (1) are different, and the specific atomic ratio composition of the finally prepared temperature measuring material is as follows: (Na)0.9Li0.1)(La0.79Gd0.1Y0.1)MgW0.98O6:Eu0.01 3+,Mn0.02 4+。
Example 7
The embodiment discloses a preparation method of a temperature measuring material based on element europium and manganese codoping, which comprises the following steps:
1) respectively weighing compounds containing elements Na, Li, La, Gd, Y, Eu, Mg, W and Mn according to the atomic ratio;
2) dissolving the nitrate in deionized water to obtain a mixed solution;
3) adding citric acid into the mixed solution under continuous stirring;
4) drying at 90 deg.C to form gel;
5) then sintering for 1-3h at 500 ℃ and sintering for 2-10h at 1000-1200 ℃ in sequence to obtain the temperature measuring material.
In some preferred embodiments of the invention, the preparation method is to co-dope the europium and the manganese elements by a sol-gel method or a high-temperature solid-phase method to prepare the temperature measuring material. The sol-gel method and the high-temperature solid phase method are conventional methods in the field.
In some preferred embodiments of the invention, the prepared thermometric material is in the form of powder, film or ceramic.
In some preferred embodiments of the invention, the emission spectrum of the temperature measuring material is detected in the temperature range of 303-523K,
in some preferred embodiments of the present invention, the compound containing elemental sodium is a mixture of one or more of oxides, hydroxides, nitrates or carbonates of sodium, and the ratio of the materials in the mixture can be arbitrarily selected.
In some preferred embodiments of the present invention, the compound containing elemental lithium is a mixture of one or more of oxides, hydroxides, nitrates or carbonates of lithium, and the ratio of the materials in the mixture can be arbitrarily selected.
In some preferred embodiments of the present invention, the compound containing elemental lanthanum is a mixture of one or more of oxides, hydroxides, nitrates or carbonates of lanthanum, and the ratio of the materials in the mixture can be arbitrarily selected.
In some preferred embodiments of the present invention, the compound containing gadolinium is a mixture of one or more of oxides, hydroxides, nitrates and carbonates of gadolinium, and the ratio of the materials in the mixture can be arbitrarily selected.
In some preferred embodiments of the present invention, the yttrium-containing compound is a mixture of one or more of yttrium oxide, hydroxide, nitrate or carbonate, and the ratio of the materials in the mixture can be arbitrarily selected.
In some preferred embodiments of the present invention, the compound containing element europium is a mixture of one or more of oxide, hydroxide, nitrate or carbonate of europium, and the ratio of the materials in the mixture can be arbitrarily selected.
In some preferred embodiments of the present invention, the compound containing elemental magnesium is a mixture of one or more of oxides, hydroxides, nitrates or carbonates of magnesium, and the ratio of the materials in the mixture can be arbitrarily selected.
In some preferred embodiments of the present invention, the compound containing elemental tungsten is a mixture of one or more of oxides, hydroxides, nitrates or carbonates of tungsten, and the ratio of each material in the mixture can be arbitrarily selected.
In some preferred embodiments of the present invention, the compound containing elemental manganese is a mixture of one or more of oxides, hydroxides, nitrates or carbonates of manganese, and the ratio of each material in the mixture can be arbitrarily selected.
It can be seen from the above embodiments that the present invention discloses a high-sensitivity temperature measuring material of a dual illuminant system doped with both rare earth europium and transition metal manganese, under effective excitation of ultraviolet light, trivalent europium Eu (iii) and tetravalent manganese Mn (iv) can simultaneously emit respective characteristic spectra as dual luminescence centers, the fluorescence intensity ratios thereof show regular changes with temperature, and can be fitted by using a standard working curve, by detecting the characteristic emission peaks with the two wavelengths far apart, a higher signal discrimination is obtained, mutual interference of detection signals is avoided, the signal detection discrimination is large, the temperature can be accurately calibrated by using the luminescence intensity ratios of the dual luminescence centers, and the temperature measuring range is wide.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A thermometric material based on co-doping of the elements europium and manganese, characterized by having an atomic ratio composition represented by the following general formula (1):
(Na1-xLix)(La1-y-z-mGdyYz)MgW1-nO6:Eum 3+,Mnn 4+(1)
wherein x, y and z satisfy the following conditions: x is more than or equal to 0 and less than or equal to 0.5, y is more than or equal to 0 and less than or equal to 0.3, and z is more than or equal to 0 and less than or equal to 0.3; m and n satisfy the following conditions: m is more than 0 and less than or equal to 0.1, and n is more than 0 and less than or equal to 0.02.
2. The thermometric material based on the codoping of the elements europium and manganese of claim 1, characterized in that said thermometric material has an atomic ratio composition represented by the following general formula (2):
(Na0.9Li0.1)(La0.75Gd0.1Y0.1)MgW0.997O6:Eu0.05 3+,Mn0.003 4+(2)
wherein x is 0.1, y is 0.1, z is 0.1, m is 0.05, and n is 0.003.
3. The thermometric material based on the codoping of the elements europium and manganese of claim 1, characterized in that said thermometric material has an atomic ratio composition represented by the following general formula (3):
(Na0.5Li0.5)(La0.35Gd0.3Y0.3)MgW0.99O6:Eu0.05 3+,Mn0.01 4+(3)
wherein x is 0.5, y is 0.3, z is 0.3, m is 0.05, and n is 0.01.
4. The thermometric material based on the codoping of the elements europium and manganese of claim 1, characterized in that said thermometric material has an atomic ratio composition represented by the following general formula (4):
(Na1.0Li0.0)(La0.95Gd0.0Y0.0)MgW0.995O6:Eu0.05 3+,Mn0.005 4+(4)
wherein x is 0.0, y is 0.0, z is 0.0, m is 0.05, and n is 0.005.
5. The thermometric material based on the co-doping of the elements europium and manganese according to claim 1, wherein the thermometric material is in the form of a powder, a film or a ceramic.
6. The method for preparing the element europium and manganese co-doped temperature measuring material of any one of claims 1 to 5, which comprises the following steps:
respectively weighing compounds containing elements Na, Li, La, Gd, Y, Eu, Mg, W and Mn according to the atomic ratio, grinding the compounds, calcining, cooling to room temperature, and grinding to obtain a temperature measuring material; or the like, or, alternatively,
respectively weighing compounds containing elements Na, Li, La, Gd, Y, Eu, Mg, W and Mn according to the atomic ratio, dissolving the compounds in water to obtain a mixed solution, adding organic acid into the mixed solution, drying to form gel, and sintering the gel to obtain the temperature measuring material.
7. The method according to claim 6, characterized in that the compound is a nitrate containing the elements Na, Li, La, Gd, Y, Eu, Mg, W and Mn.
8. The method of claim 6, wherein the organic acid is citric acid.
9. A method for obtaining a temperature measurement of an environment to be measured by using the thermometric material of any one of claims 1-5, comprising the steps of:
step one, testing emission spectra of temperature measuring materials at different temperatures, and establishing a standard working curve of integral luminous intensity ratio of trivalent europium Eu (III) emission peak and tetravalent manganese Mn (IV) emission peak along with temperature change;
placing the temperature measuring material in a temperature environment to be measured, and measuring the emission spectrum of the temperature measuring material to further obtain the integral luminous intensity ratio of the emission peak of trivalent europium Eu (III) and the emission peak of tetravalent manganese Mn (IV);
and step three, obtaining the temperature measurement value of the environment to be measured through a standard working curve according to the integral luminous intensity ratio of the environment to be measured.
10. The method of claim 9, wherein the integrated luminescence intensity ratio with absolute temperature satisfies the following exponential equation:
FIR＝IEu3+/IMn4+＝A×exp(B/T)+C；
wherein FIR is the ratio of integrated luminous intensity, T is absolute temperature, IEu3+And IMn4+The integrated luminescence intensities of the emission peaks of trivalent europium Eu (III) and tetravalent manganese Mn (IV), A, B, C are constants respectively.
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| CN113403075A (en) * | 2021-05-28 | 2021-09-17 | 杭州电子科技大学 | Mn (manganese)4+-Sm3+Co-doped antimonate fluorescent temperature probe material and preparation method and application thereof |
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| CN112175619A (en) * | 2020-10-30 | 2021-01-05 | 东台市天源光电科技有限公司 | LED plant growth warm white light fluorescent powder and preparation method thereof |
| CN113292998A (en) * | 2021-05-28 | 2021-08-24 | 杭州电子科技大学 | Double-activated ion doped double-perovskite type fluorescent temperature probe material and preparation method and application thereof |
| CN113403075A (en) * | 2021-05-28 | 2021-09-17 | 杭州电子科技大学 | Mn (manganese)4+-Sm3+Co-doped antimonate fluorescent temperature probe material and preparation method and application thereof |
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