Yellow fluorescence temperature measurement material based on Eu < 2 + > half-peak width and preparation and application thereof

Abstract

The invention relates to the technical field of fluorescent temperature measurement sensing, in particular to a yellow fluorescent temperature measurement material based on Eu < 2 + > half-peak width and preparation and application thereof. In the invention, the chemical expression of the fluorescent temperature measurement material is Ba3Sc2B4O12: xEu < 2 + >, and x is more than or equal to 0.01 and less than or equal to 0.05. The material is prepared through a high-temperature solid-phase method, and a variable-temperature spectrum within the temperature range of 298-473K is obtained by exciting the material by adopting 338nm as an excitation light source. When Eu < 2 + > is doped, the temperature is measured by using the change of the half-peak width value of Eu < 2 + >, and the obtained maximum absolute temperature sensitivity and relative temperature sensitivity can reach 0.17 K <-1 > and 0.11% K <-1 >.

Description

Technical Field

[0001] The present invention relates to the technical field of fluorescence temperature sensing, and in particular to a yellow fluorescence temperature sensing material based on the full width at half maximum (FWHM) of Eu, and its preparation and application. 2+ Background Art

[0002] Accurate temperature measurement has a wide range of applications in many fields such as environmental monitoring, industrial production, military and national defense. Traditional contact temperature measurement requires the sensor element of the thermometer to have mechanical thermal contact with the temperature measurement medium. The instrument is generally simple and reliable, but there are some inevitable disadvantages, such as being easily affected by strong electromagnetic noise interference, not being suitable for special environments such as strongly corrosive atmospheres and strong magnetic fields, and having a long response time. However, due to the effective overcoming of the above defects, non-contact optical temperature sensors based on optical response have received extensive attention. According to the main luminescence parameters such as the emission bandwidth, fluorescence intensity ratio, emission peak position, and fluorescence lifetime of the phosphor, the temperature can be conveniently and rapidly measured. Among them, the non-contact temperature measurement technology based on the full width at half maximum (FWHM) technology has received extensive attention due to its advantages of fast response, self-reference, and being unaffected by power fluctuations and spectral losses. Therefore, developing a high-precision and high-sensitivity optical temperature sensor based on the emission bandwidth modulation of Eu-doped luminescent materials is of great significance for further exploring non-contact optical temperature measurement. 2+ Summary of the Invention

[0003] In order to solve the above problems, the purpose of the present invention is to provide a yellow fluorescence temperature sensing material based on the full width at half maximum (FWHM) of Eu, and its preparation and application. The yellow fluorescence temperature sensing material based on the full width at half maximum (FWHM) of Eu provided by the present invention can utilize the full width at half maximum (FWHM) of Eu to achieve high-sensitivity temperature measurement, meeting the current urgent need for high-sensitivity non-contact optical temperature measurement. 2+ 2+ 2+

[0004] The purpose of the present invention can be achieved by the following technical solutions:

[0005] The first purpose of the present invention is to provide a yellow fluorescence temperature sensing material based on the full width at half maximum (FWHM) of Eu. The chemical expression of the fluorescence material is Ba3Sc2B4O 2+ :xEu 12 2+ where 0.01 ≤ x ≤ 0.05.

[0006] In an embodiment of the present invention, x is 0.01, 0.02, 0.03, 0.04 or 0.05;

[0007] Preferably, x is 0.03.

[0008] In one embodiment of the present invention, the emission wavelength of the fluorescent temperature - measuring material is 575 nm, and the absolute sensitivity is 0.17 K -1 , and the relative sensitivity is 0.12% K -1 .

[0009] The yellow fluorescent temperature - measuring material provided by the present invention is a brand - new, unreported Eu 2+ - doped borate - based 575 - nm yellow - light - emitting fluorescent material. The phosphor has a wide emission spectrum, and at the same time, the phosphor has high thermal quenching performance and is significantly affected by temperature. The yellow fluorescent temperature - measuring material provided by the present invention can be prepared by a conventional solid - state reaction method, has the characteristics of simple preparation process and is conducive to industrial production, and can be used as a good candidate material for wide application of non - contact optical temperature measurement.

[0010] The second object of the present invention is to provide a preparation method of a yellow fluorescent temperature - measuring material based on the full - width at half - maximum (FWHM) of Eu 2+ , comprising the following steps:

[0011] (1) Mix a barium - source compound, a scandium - source compound, a boron - source compound, and an europium - source compound to obtain a mixed material;

[0012] (2) Grind and mix the mixed material obtained in step (1) to obtain raw material powder;

[0013] (3) Sinter the ground raw material powder obtained in step (2), and then cool it to room temperature to finally obtain the yellow fluorescent temperature - measuring material based on the full - width at half - maximum (FWHM) of Eu 2+ .

[0014] In one embodiment of the present invention, in step (1), the barium - source compound is a barium - containing carbonate;

[0015] the scandium - source compound is a scandium - containing oxide;

[0016] the boron - source compound is a boron - containing oxide;

[0017] the europium - source compound is a europium - containing oxide.

[0018] In one embodiment of the present invention, the barium - source compound is BaCO3, the scandium - source compound is Sc2O3, the boron - source compound is H3BO3, and the europium - source compound is Eu2O3.

[0019] In one embodiment of the present invention, in step (2), during the grinding process, the time is 10 - 120 min.

[0020] In one embodiment of the present invention, in step (3), the calcination process is carried out in a reducing atmosphere, with a pressure of 0 MPa, a temperature of 900 - 1200 °C, and a time of 4 - 10 h.

[0021] Preferably, during the calcination process, the temperature is 900 - 960 °C and the time is 8 h.

[0022] In one embodiment of the present invention, the method of high-temperature sintering is specifically as follows: Load the raw material powder into an alumina crucible, and then place the alumina crucible containing the raw materials in a reducing atmosphere for sintering.

[0023] In one embodiment of the present invention, the reducing atmosphere is selected from a mixed gas of H2 and N2.

[0024] Preferably, the reducing atmosphere is selected from a mixed gas of 5% by volume of H2 and 95% by volume of N2.

[0025] The third object of the present invention is to provide an application of a yellow fluorescent temperature measurement material based on the full width at half maximum of Eu 2+ in the preparation of a non-contact optical temperature measurement device.

[0026] Eu ions with a 4f-5d electronic configuration 2+ are excellent activators for phosphors. Due to the 4f-5d transition of Eu 2+ , Eu 2 + can easily exhibit a broad and effective emission band. Compared with the sharp emission peaks of rare earth ions with 4f-4f transitions, the broadband emission of Eu 2+ ions has greater peak stability, a shorter decay lifetime, and a faster thermodynamic response speed.

[0027] Accurate temperature measurement has a wide range of applications in environmental monitoring, industrial production, military and defense industries, and many other fields. Traditional contact temperature measurement requires mechanical thermal contact between the sensor element of the thermometer and the temperature measurement medium. This instrument is usually simple and reliable, but it also has some inevitable disadvantages, such as being vulnerable to strong electromagnetic noise interference, not being suitable for special environments such as highly corrosive atmospheres and strong magnetic fields, and having a long response time. However, non-contact optical temperature sensors based on optical response have received extensive attention because they can effectively overcome the disadvantages of traditional contact temperature measurement. Using key luminescence parameters of phosphors, such as emission bandwidth, fluorescence intensity ratio (FIR), emission peak position, and fluorescence lifetime, temperature can be measured accurately and quickly. Currently, the main method of optical temperature measurement relies on FIR. However, optical temperature sensing phosphors usually undergo thermal quenching at high temperatures, which introduces noise interference in the intensity signal, thereby reducing the measurement accuracy and precision. In contrast, the emission bandwidth of the fluorescence peak is insensitive to external interferences such as light source fluctuations and excitation power drift. At the same time, due to the enhanced electron-phonon interaction, the emission bandwidth usually increases with the increase in temperature. This correlation indicates that optical temperature measurement based on full width at half maximum (FWHM) is a feasible alternative, such as YOF:Yb 3+ / Tm 3+ reported by Lu Hongyu and LiGa4(MgGe) 0.5 O8:Cr 3+ reported by Wang Yuzhen. Compared with narrowband transmission, broadband transmission shows significantly stronger anti-interference ability. Therefore, this application innovatively proposes an optical temperature measurement strategy based on the analysis of the full width at half maximum of broadband emission phosphors. In lighting technology, this kind of broadband phosphor has become a key material due to its excellent spectral tunability and excellent color rendering ability. The above characteristics enable the developed phosphor to simultaneously address two key technical challenges: promoting the application of white LEDs with high color rendering index, and achieving high-precision non-contact temperature sensing through the detection mode based on full width at half maximum.

[0028] This invention will select Eu 2+ as the luminescence center of the phosphor, select Ba3Sc2B4O 12 as the matrix material, and synthesize a high-precision and high-sensitivity fluorescence temperature measurement material Ba 3-x Sc2B4O 12 :xEu 2+ . By fitting the full width at half maximum values of this material at different temperatures, the absolute sensitivity S a and the relative sensitivity S r can be calculated. In the range of 298 - 473K, the S 3-x Sc2B4O 122 :xEu 2+ of S a and S rAll decrease with increasing temperature. At 298 K, S a and S r reach their maximum values, where S a(max) = 0.17 K -1 , S r(max) = 0.12% K -1 . Compared with the reported optical temperature - measuring materials, this material has a relatively large absolute sensitivity. Ba 3-x Sc2B4O 122 :xEu 2+ phosphor has great potential in optical temperature detection.

[0029] Compared with the prior art, the present invention has the following beneficial effects:

[0030] (1) The phosphor of the present invention has a wide emission band, covering the range of 450 - 820 nm, and the full - width at half - maximum at room temperature can reach 144 nm.

[0031] (2) The phosphor of the present invention is prepared by a conventional solid - state reaction method, has the characteristics of simple preparation process and is conducive to industrial production. It can be used as a good candidate material for wide application of non - contact optical temperature - measuring devices, and has broad application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 are the XRD patterns of the yellow fluorescent temperature - measuring materials based on Eu 2+ full - width at half - maximum prepared in Example 1, Example 2, Example 3, Example 4 and Example 5;

[0033] Figure 2 is the variable - temperature spectrum of the yellow fluorescent temperature - measuring material based on Eu 2+ full - width at half - maximum - Ba 2.97 Sc2B4O 122 :0.03Eu 2+ under near - ultraviolet excitation prepared in Example 1;

[0034] Figure 3 is the relationship diagram of the full - width at half - maximum of Eu 2+ in the yellow fluorescent temperature - measuring material based on Eu 2.97 Sc2B4O 122 :0.03Eu 2+ changing with temperature prepared in Example 1; 2+

[0035] Figure 4 is the yellow fluorescent temperature - measuring material based on Eu 2+ full - width at half - maximum - Ba 2.97 Sc2B4O 122 :0.03Eu2+ Graph of the dependence of relative and absolute sensitivity on temperature Detailed implementation manners

[0036] The present invention provides a yellow fluorescent temperature - measuring material based on Eu 2+ with a full - width at half - maximum, and the chemical formula of the fluorescent material is Ba3Sc2B4O 12 :xEu 2+ , where 0.01 ≤ x ≤ 0.05

[0037] Furthermore, x is 0.01, 0.02, 0.03, 0.04 or 0.05

[0038] Preferably, x is 0.03

[0039] Furthermore, the emission wavelength of the fluorescent temperature - measuring material is 575 nm, the absolute sensitivity is 0.17 K -1 , and the relative sensitivity is 0.12% / K -1 .

[0040] The yellow fluorescent temperature - measuring material provided by the present invention is a brand - new Eu 2+ - doped borate - based 575 - nm yellow - light - emitting fluorescent material. The fluorescent powder has a wide emission spectrum, and at the same time, the fluorescent powder has high thermal quenching performance and is significantly affected by temperature. The yellow fluorescent temperature - measuring material provided by the present invention can be prepared by a conventional solid - state reaction method, has the characteristics of simple preparation process and being conducive to industrial production, and can be used as a good candidate material for wide application of non - contact optical temperature measurement

[0041] The present invention provides a preparation method of a yellow fluorescent temperature - measuring material based on Eu 2+ with a full - width at half - maximum, comprising the following steps

[0042] (1) Mixing a barium - source compound, a scandium - source compound, a boron - source compound, and an europium - source compound to obtain a mixed material

[0043] (2) Grinding and mixing the mixed material obtained in step (1) to obtain raw material powder

[0044] (3) Sintering the ground raw material powder obtained in step (2), and then cooling to room temperature to finally obtain the yellow fluorescent temperature - measuring material based on Eu 2+ with a full - width at half - maximum

[0045] Furthermore, in step (1), the barium - source compound is a barium - containing carbonate

[0046] The scandium - source compound is a scandium - containing oxide

[0047] The boron source compound is a boron-containing oxide;

[0048] The europium source compound is a europium-containing oxide.

[0049] Furthermore, the barium source compound is BaCO3, the scandium source compound is Sc2O3, the boron source compound is H3BO3, and the europium source compound is Eu2O3.

[0050] Furthermore, in step (2), during the grinding process, the time is 10 to 120 minutes.

[0051] Furthermore, in step (3), the calcination process is carried out in a reducing atmosphere, the pressure is 0 MPa, the temperature is 900 to 1200 °C, and the time is 4 to 10 hours.

[0052] Preferably, during the calcination process, the temperature is 900 to 960 °C and the time is 8 hours.

[0053] Furthermore, the method of high-temperature sintering is as follows: Load the raw material powder into an alumina crucible, and then place the alumina crucible containing the raw materials in a reducing atmosphere for sintering.

[0054] Furthermore, the reducing atmosphere is selected from a mixed gas of H2 and N2.

[0055] Preferably, the reducing atmosphere is selected from a mixed gas of 5% by volume of H2 and 95% by volume of N2.

[0056] The present invention provides an application of a yellow fluorescent temperature measurement material based on Eu 2+ with a full width at half maximum in the preparation of a non-contact optical temperature measurement device.

[0057] The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.

[0058] In the following examples, unless otherwise specified, the reagents used are commercially available reagents, and the detection means and methods used are conventional detection means and methods in the art.

[0059] Example 1

[0060] This example provides a preparation method of a yellow fluorescent temperature measurement material based on Eu 2+ with a full width at half maximum, specifically including the following steps:

[0061] (1) Weigh 1 g of raw material powders of BaCO3, Sc2O3, H3BO3, and Eu2O3 according to the stoichiometric ratio (the mass ratio of each raw material is BaCO3:Sc2O3:H3BO3:Eu2O3 = 0.5887:0.1413:0.2535:0.0162) to obtain a mixed material.

[0062] (2) Place the mixture obtained in step (1) in an agate mortar and grind it for 40 minutes. After the materials are evenly mixed, load the mixture into an alumina crucible, place it in a reducing atmosphere of a hydrogen-nitrogen mixture (a mixed gas of 5% by volume of H2 and 95% by volume of N2), and calcine it at 960 °C for 8 h with a heating rate of 5 °C / h. Then cool it to room temperature to obtain the target product: yellow fluorescence temperature measurement material based on Eu 2+ with a full width at half maximum - Ba 2.97 Sc2B4O 122 :0.03Eu 2+ (hereinafter also abbreviated as "BSBO:0.03Eu 2+ ").

[0063] Perform phase analysis on the target product prepared in this example, and the obtained XRD pattern is as shown in Figure 1 Ba in 2.97 Sc2B4O 122 :0.03Eu 2+ shown. Compared with the standard PDF card, the diffraction peak positions and diffraction intensities correspond one by one. It can be found through Figure 1 that the doping of Eu 2+ on the surface does not introduce impurities, proving that the pure-phase rare-earth doped fluorescence temperature measurement material was successfully synthesized in this example.

[0064] Performance analysis:

[0065] Place the fluorescence temperature measurement material prepared in this example in a test device, use incident light with a central wavelength of 338 nm to excite it, and obtain a variable-temperature spectrum as shown in Figure 2 shown. As the temperature increases, the emission intensity of BSBO:0.03Eu 2+ decreases due to the quenching effect; and the full width at half maximum of the emission band is significantly affected by temperature. In the temperature range of 298 K to 483 K, due to the significant enhancement of the electron-phonon interaction, the full width at half maximum value of the emission band shows a significant increasing trend. The full width at half maximum values at different temperatures can be fitted using a simplified formula:

[0066] v = A + B * exp(C * T) Formula (1);

[0067] where the parameters A, B, and C in the formula are all coefficients.

[0068] According to Formula (1), the full width at half maximum values of BSBO:0.03Eu 2+ in the range of 298 K to 483 K were calculated, and a curve of temperature versus full width at half maximum value was obtained, and the result is as shown in Figure 3As shown in the figure, the fitting equation is FWHM=212-50exp[-0.0025(T-419)], and the fitting degree is 0.991. All the half-peak width fitting results match the formula well. In addition, the relative sensitivity (S r ) and absolute sensitivity (S a ) can determine the sensing performance (such as Figure 4 Differentiate the fitting function and get the formula:

[0069]

[0070]

[0071] Using formula (2) (3), calculate Ba 3-x Sc2B4O 12 :0.03Eu 2+ S in the range of 298-473K a and S r In the temperature range of 298K~473K, S a and S r It shows a downward trend and reaches a maximum value at 298K, which is 0.17K -1 and 0.12% K -1 Compared with other temperature measurement materials studied in the past, as shown in Table 1, the phosphors based on FWHM show lower S at high temperatures. r value; however, phosphors used for optical temperature sensing often undergo thermal quenching at high temperatures, which impairs the noise resistance of the luminescence intensity signal, thereby reducing the measurement precision and accuracy of intensity-based optical temperature measurement. In contrast, the emission bandwidth of the fluorescence peak is insensitive to external interference such as light source fluctuations and excitation power drift, and has excellent signal stability and accuracy. A wider half-maximum full width can further improve the efficiency of optical signal collection, while minimizing noise interference in the temperature measurement equipment, significantly improving the operational reliability of the temperature measurement equipment.

[0072] Table 1 Relative sensitivity of typical phosphors in the prior art

[0073]

[0074] Example 2

[0075] This embodiment provides a method based on Eu 2+ The preparation method of the half-width yellow fluorescent temperature measuring material specifically comprises the following steps:

[0076] (1) Weigh 1 g of raw material powders of BaCO3, Sc2O3, H3BO3, and Eu2O3 according to the stoichiometric ratio to obtain a mixture.

[0077] (2) Grind the mixture obtained in step (1) in an agate mortar for 40 minutes. After the materials are evenly mixed, load the mixture into an alumina crucible, and place it in a reducing atmosphere of hydrogen-nitrogen mixture (a mixed gas of 5% by volume of H2 and 95% by volume of N2) for calcination at 960 °C for 8 h, with a heating rate of 5 °C / h. Then cool it to room temperature to obtain the target product: yellow fluorescence temperature measurement material - Ba 2+ Based on the full width at half maximum - Ba 2.99 Sc2B4O 122 :0.01Eu 2+ (Compared with Example 1, only the raw material ratios are different; its XRD pattern is as shown in Figure 1 ).

[0078] Example 3

[0079] This example provides a preparation method of a yellow fluorescence temperature measurement material based on Eu 2+ Based on the full width at half maximum, which specifically includes the following steps:

[0080] (1) Weigh 1 g of raw material powders of BaCO3, Sc2O3, H3BO3, and Eu2O3 according to the stoichiometric ratio to obtain a mixture.

[0081] (2) Grind the mixture obtained in step (1) in an agate mortar for 40 minutes. After the materials are evenly mixed, load the mixture into an alumina crucible, and place it in a reducing atmosphere of hydrogen-nitrogen mixture (a mixed gas of 5% by volume of H2 and 95% by volume of N2) for calcination at 960 °C for 8 h, with a heating rate of 5 °C / h. Then cool it to room temperature to obtain the target product: yellow fluorescence temperature measurement material - Ba 2+ Based on the full width at half maximum - Ba 2.98 Sc2B4O 122 :0.02Eu 2+ (Compared with Example 1, only the raw material ratios are different; its XRD pattern is as shown in Figure 1 ).

[0082] Example 4

[0083] This example provides a preparation method of a yellow fluorescence temperature measurement material based on Eu 2+ Based on the full width at half maximum, which specifically includes the following steps:

[0084] (1) Weigh 1 g of raw material powders of BaCO3, Sc2O3, H3BO3, and Eu2O3 according to the stoichiometric ratio to obtain a mixture.

[0085] (2) Grind the mixture obtained in step (1) in an agate mortar for 40 minutes. After the materials are evenly mixed, load the mixture into an alumina crucible and place it in a reducing atmosphere of a hydrogen-nitrogen mixture (a mixed gas of 5% by volume of H2 and 95% by volume of N2) for calcination at 960 °C for 8 h. The heating rate is 5 °C / h, and then cool it to room temperature to obtain the target product: yellow fluorescence temperature measurement material based on Eu 2+ Full-width at half-maximum yellow fluorescence temperature measurement material - Ba 2.96 Sc2B4O 122 :0.04Eu 2+ (Compared with Example 1, only the ratios of each raw material are different; its XRD pattern is as Figure 1 shown).

[0086] Example 5

[0087] This example provides a preparation method of a yellow fluorescence temperature measurement material based on Eu 2+ Full-width at half-maximum, which specifically includes the following steps:

[0088] (1) Weigh 1 g of raw material powders of BaCO3, Sc2O3, H3BO3, and Eu2O3 according to the stoichiometric ratio to obtain a mixture.

[0089] (2) Grind the mixture obtained in step (1) in an agate mortar for 40 minutes. After the materials are evenly mixed, load the mixture into an alumina crucible and place it in a reducing atmosphere of a hydrogen-nitrogen mixture (a mixed gas of 5% by volume of H2 and 95% by volume of N2) for calcination at 960 °C for 8 h. The heating rate is 5 °C / h, and then cool it to room temperature to obtain the target product: yellow fluorescence temperature measurement material based on Eu 2+ Full-width at half-maximum yellow fluorescence temperature measurement material - Ba 2.95 Sc2B4O 122 :0.05Eu 2+ (Compared with Example 1, only the ratios of each raw material are different; its XRD pattern is as Figure 1 shown).

[0090] Example 6

[0091] This example provides a preparation method of a yellow fluorescence temperature measurement material based on Eu 2+ Full-width at half-maximum, which specifically includes the following steps:

[0092] (1) Weigh 1 g of raw material powders of BaCO3, Sc2O3, H3BO3, and Eu2O3 according to the stoichiometric ratio (the mass ratio of each raw material is BaCO3:Sc2O3:H3BO3:Eu2O3 = 0.5887:0.1413:0.2535:0.0162) to obtain a mixture.

[0093] (2) Grind the mixture obtained in step (1) in an agate mortar for 40 minutes. After the materials are evenly mixed, load the mixture into an alumina crucible and place it in a reducing atmosphere of hydrogen-nitrogen mixture (a mixed gas of 5% by volume of H2 and 95% by volume of N2) for calcination at 900 °C for 6 h, with a heating rate of 5 °C / h. Then cool it to room temperature to obtain the target product: yellow fluorescent temperature-measuring material - Ba 2+ with a half-peak width based on Eu 2.97 Sc2B4O 122 :0.03Eu 2+ .

[0094] Example 7

[0095] This example provides a preparation method of a yellow fluorescent temperature-measuring material based on Eu 2+ with a half-peak width, specifically including the following steps:

[0096] (1) Weigh 1 g of raw material powders of BaCO3, Sc2O3, H3BO3, and Eu2O3 according to the stoichiometric ratio (the mass ratio of each raw material is BaCO3: Sc2O3: H3BO3: Eu2O3 = 0.5887: 0.1413: 0.2535: 0.0162) to obtain a mixture.

[0097] (2) Grind the mixture obtained in step (1) in an agate mortar for 40 minutes. After the materials are evenly mixed, load the mixture into an alumina crucible and place it in a reducing atmosphere of hydrogen-nitrogen mixture (a mixed gas of 5% by volume of H2 and 95% by volume of N2) for calcination at 940 °C for 4 h, with a heating rate of 5 °C / h. Then cool it to room temperature to obtain the target product: yellow fluorescent temperature-measuring material - Ba 2+ with a half-peak width based on Eu 2.97 Sc2B4O 122 :0.03Eu 2+ .

[0098] The performance of the yellow fluorescent temperature-measuring materials prepared in Examples 2 - 7 is slightly worse than that of the yellow fluorescent temperature-measuring material prepared in Example 1.

[0099] Example 8

[0100] This example provides a preparation method of a yellow fluorescent temperature-measuring material based on Eu 2+ with a half-peak width, specifically including the following steps:

[0101] (1) Weigh 1 g of raw material powders of BaCO3, Sc2O3, H3BO3, and Eu2O3 according to the stoichiometric ratio (the mass ratio of each raw material is BaCO3:Sc2O3:H3BO3:Eu2O3 = 0.5887:0.1413:0.2535:0.0162) to obtain a mixed material.

[0102] (2) Place the mixed material obtained in step (1) in an agate mortar and grind it for 40 minutes. After the materials are mixed evenly, load the mixture into an alumina crucible, place it in a reducing atmosphere of a hydrogen-nitrogen mixture (a mixed gas of 5% by volume of H2 and 95% by volume of N2), and calcine it at 1000 °C for 4 h with a heating rate of 5 °C / h. Then cool it to room temperature to obtain the target product: a yellow fluorescent temperature measurement material based on Eu 2+ Full width at half maximum - Ba 2.97 Sc2B4O 122 :0.03Eu 2+ .

[0103] Example 9

[0104] This example provides a preparation method for a yellow fluorescent temperature measurement material based on Eu 2+ Full width at half maximum, specifically including the following steps:

[0105] (1) Weigh 1 g of raw material powders of BaCO3, Sc2O3, H3BO3, and Eu2O3 according to the stoichiometric ratio (the mass ratio of each raw material is BaCO3:Sc2O3:H3BO3:Eu2O3 = 0.5887:0.1413:0.2535:0.0162) to obtain a mixed material.

[0106] (2) Place the mixed material obtained in step (1) in an agate mortar and grind it for 40 minutes. After the materials are mixed evenly, load the mixture into an alumina crucible, place it in a reducing atmosphere of a hydrogen-nitrogen mixture (a mixed gas of 5% by volume of H2 and 95% by volume of N2), and calcine it at 1000 °C for 4 h with a heating rate of 5 °C / h. Then cool it to room temperature to obtain the target product: a yellow fluorescent temperature measurement material based on Eu 2+ Full width at half maximum - Ba 2.97 Sc2B4O 122 :0.03Eu 2+ .

[0107] Example 10

[0108] This example provides a preparation method for a yellow fluorescent temperature measurement material based on Eu 2+ Full width at half maximum, specifically including the following steps:

[0109] (1) Weigh 1 g of raw material powders of BaCO3, Sc2O3, H3BO3, and Eu2O3 according to the stoichiometric ratio (the mass ratio of each raw material is BaCO3:Sc2O3:H3BO3:Eu2O3 = 0.5887:0.1413:0.2535:0.0162) to obtain a mixed material.

[0110] (2) Place the mixed material obtained in step (1) in an agate mortar and grind it for 40 minutes. After the materials are mixed evenly, load the mixture into an alumina crucible, place it in a reducing atmosphere of a hydrogen-nitrogen mixture (a mixed gas of 5% by volume of H2 and 95% by volume of N2), and calcine it at 1200 °C for 6 h with a heating rate of 5 °C / h. Then cool it to room temperature to obtain the target product: yellow fluorescence temperature measurement material - Ba 2+ based on the full width at half maximum of Eu 2.97 Sc2B4O 122 :0.03Eu 2+ .

[0111] The performance of the yellow fluorescence temperature measurement materials prepared in Examples 8 - 10 is slightly worse than that of the yellow fluorescence temperature measurement material prepared in Example 1.

[0112] Comparative Example 1

[0113] This comparative example provides a preparation method of a yellow fluorescence temperature measurement material based on the full width at half maximum of Eu 2+ . Compared with Example 1, this example is the same as Example 1 in all aspects except for the following differences:

[0114] The chemical structural formula of the yellow fluorescence temperature measurement material is Ba 2.99 Sc2B4O 122 :0.01Eu 2+ .

[0115] The maximum value of S 2.99 Sc2B4O 122 :0.01Eu 2+ in the range of 298 - 473 K is 0.15 K a ; the maximum value of the S -1 value is 0.10% K r . -1 .

[0116] This is because the doping concentration in this comparative example is not the optimal one, and both the emission intensity and the emission bandwidth are worse than those in Example 1. Therefore, the calculated S a , S r are both lower than those in Example 1.

[0117] Comparative Example 2

[0118] This embodiment provides a preparation method of a fluorescence temperature measurement material, which specifically includes the following steps:

[0119] (1) Weigh 1 g of raw material powders of BaCO3, Sc2O3, H3BO3, and Eu2O3 according to the stoichiometric ratio (the mass ratio of each raw material is BaCO3: Sc2O3: H3BO3: Eu2O3 = 0.5887: 0.1413: 0.2535: 0.0162) to obtain a mixture.

[0120] (2) Place the mixture obtained in step (1) in an agate mortar and grind it for 40 minutes. After the materials are mixed evenly, load the mixture into an alumina crucible, place it in a reducing atmosphere of a hydrogen-nitrogen mixture (a mixed gas of 5% by volume of H2 and 95% by volume of N2), and calcine it at 1300 °C for 6 h with a heating rate of 5 °C / h. Then cool it to room temperature to obtain the target product: fluorescence temperature measurement material - Ba 2.97 Sc2B4O 122 :0.03Eu 2+ .

[0121] The maximum value of S of the Ba 2.97 Sc2B4O 122 :0.03Eu 2+ prepared in this comparative example within the range of 298 - 473 K is 0.11 K a ; the maximum value of the S -1 value is 0.09% K r . -1 .

[0122] This may be because the sample prepared under this synthesis condition is not a pure phase and there are impurity phases, which affect spectral properties such as emission bandwidth and emission intensity. Therefore, the calculated S a , S r are both lower than those in Example 1.

[0123] The above description of the embodiments is for the convenience of those of ordinary skill in the art to understand and use the invention. Those who are familiar with the technology in this field can obviously make various modifications to these embodiments easily and apply the general principles described here to other embodiments without creative labor. Therefore, the present invention is not limited to the above embodiments, and the improvements and modifications made by those skilled in the art without departing from the scope of the present invention according to the disclosure of the present invention should be within the protection scope of the present invention.

Claims

1. A yellow fluorescence temperature measurement material based on Eu 2+ , characterized in that The chemical formula of the fluorescent material is Ba3Sc2B4O 12 :xEu 2+ , where 0.01 ≤ x ≤ 0.05; The emission wavelength of the fluorescence temperature measurement material is 575 nm, and the absolute sensitivity is 0.17 K -1 , and the relative sensitivity is 0.11% K -1 .

2. A yellow fluorescent temperature measuring material based on Eu according to claim 1 2+ with a full width at half maximum, characterized in that x is 0.01, 0.02, 0.03, 0.04 or 0.

05.

3. A preparation method of a yellow fluorescence temperature measurement material based on Eu as described in any one of claims 1 to 2 2+ with a half-peak width, characterized in that It includes the following steps: (1) Mix a barium source compound, a scandium source compound, a boron source compound and a europium source compound to obtain a mixed material; (2) Grind and mix the mixed material obtained in step (1) to obtain raw material powder; (3) Sinter the ground raw material powder obtained in step (2), and then cool it to room temperature to finally obtain the yellow fluorescent temperature measuring material based on Eu 2+ with a full width at half maximum.

4. A preparation method of a yellow fluorescence temperature measurement material based on Eu according to claim 3 2+ , characterized in that In step (1), the barium source compound is a barium-containing carbonate; The scandium source compound is a scandium-containing oxide; The boron source compound is a boron-containing oxide; The europium source compound is a europium-containing oxide.

5. A preparation method of a yellow fluorescent temperature measuring material based on Eu 2+ with a full width at half maximum, characterized in that The barium source compound is BaCO3, the scandium source compound is Sc2O3, the boron source compound is H3BO3, and the europium source compound is Eu2O3.

6. A preparation method of a yellow fluorescence temperature measurement material based on Eu according to claim 3, characterized in that 2+ the full width at half maximum In step (2), during the grinding process, the time is 10 to 120 minutes.

7. A preparation method of a yellow fluorescence temperature measurement material based on Eu 2+ with a half-peak width, characterized in that In step (3), the calcination process is carried out in a reducing atmosphere, the pressure is 0 MPa, the temperature is 900 to 1200 °C, and the time is 4 to 10 hours.

8. A preparation method of a yellow fluorescence temperature measuring material based on Eu according to claim 7 2+ , characterized in that In step (3), during the calcination process, the temperature is 900 to 960 °C and the time is 8 hours.

9. A preparation method of a yellow fluorescence temperature measurement material based on Eu with a 2+ full width at half maximum, characterized in that The reducing atmosphere is selected from a mixed gas of H2 and N2.

10. Use of a yellow fluorescence temperature measuring material based on Eu with a full width at half maximum as described in any one of claims 1 to 2 in the preparation of a non-contact optical temperature measuring device. 2+ The application of the yellow fluorescence temperature measuring material with a full width at half maximum in the preparation of a non-contact optical temperature measuring device.

Images