CN115093853A - Fluorescent powder Ba with negative thermal quenching behavior 3 Eu 1-x RE x Al 2-y M y O 7.5 And method for preparing the same - Google Patents
Fluorescent powder Ba with negative thermal quenching behavior 3 Eu 1-x RE x Al 2-y M y O 7.5 And method for preparing the same Download PDFInfo
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Abstract
The invention discloses a fluorescent powder Ba with negative thermal quenching behavior 3 Eu 1‑x RE x Al 2‑y M y O 7.5 The preparation method belongs to the field of inorganic luminescent materials, wherein RE is one of La, Lu, Y and Gd, and M is Ga or Si; when x is 0, y is 0.01-0.02; when y is 0, x is 0.01-0.05; the preparation method is characterized by comprising the steps of preparing by a high-temperature solid phase method, weighing raw materials according to a proportion, adding absolute ethyl alcohol, stirring, standing, drying, pressing the obtained wafer, sintering the wafer in a high-temperature muffle furnace at 1400-1500 ℃ for 250-420 min to obtain monoclinic fluorescent powder, emitting stronger orange red light under the excitation of UV/NUV light, and showing obvious negative thermal quenching behavior at 30-300 ℃, namely obviously enhancing the luminous intensity along with the increase of the temperature.
Description
Technical Field
The invention belongs to the field of inorganic luminescent materials, and particularly relates to fluorescent powder Ba with negative thermal quenching behavior 3 Eu 1- x RE x Al 2-y M y O 7.5 And a method for preparing the same.
Background
Inorganic luminescent materials activated by trivalent rare earth ions can emit light of different wave bands under the excitation of light, and play an important role in different fields according to the performance of the materials. Wherein the thermal quenching is one of the important parameters for evaluating the thermal stability of the fluorescent powder. Most fluorescent materials exhibit varying degrees of thermal quenching, i.e., the intensity of luminescence decreases with increasing temperature. This is due to the fact that the probability of radiationless relaxation increases with increasing temperature, resulting in a large loss of energy and a decrease in emission intensity. Therefore, these phosphors also have a problem that the color of emitted light is unstable in practical use. These drawbacks can severely limit the application and development fields of phosphors. Therefore, the development of the fluorescent powder with simple preparation method, stable luminescence property and excellent thermal stability has very important practical significance.
Disclosure of Invention
To solve the above problems, the present invention provides a phosphor Ba having a negative thermal quenching behavior 3 Eu 1-x RE x Al 2-y M y O 7.5 And a method for preparing the same.
The technical scheme adopted by the invention is as follows:
fluorescent powder Ba with negative thermal quenching behavior 3 Eu 1-x RE x Al 2-y M y O 7.5 Characterized in that it belongs to the monoclinic system, space group is P2/c, unit cell parameters are
Wherein RE is one of La, Lu, Y and Gd, and M is Ga or Si; when x is 0, y is 0.01-0.02; when y is 0, x is 0.01 to 0.05.
Further, the phosphor Ba 3 Eu 1-x RE x Al 2-y M y O 7.5 Under the excitation of UV-NUV (ultraviolet-near ultraviolet) light, the material has negative thermal quenching behavior at the temperature of 30-300 ℃.
Phosphor Ba having negative thermal quenching behavior 3 Eu 1-x RE x Al 2-y M y O 7.5 The preparation method is characterized by comprising the following steps:
step 1: according to the mole of elements of Ba, Eu, RE, Al and MThe ratio is 3: (1-x): x: (2-y): weighing the raw material BaCO according to the proportion of y 3 、Eu 2 O 3 、RE 2 O 3 、Al(OH) 3 And M 2 O 3 (ii) a Wherein RE is one of La, Lu, Y and Gd, and M is Ga or Si; when x is 0, y is 0.01-0.02; when y is 0, x is 0.01-0.05;
step 2: adding absolute ethyl alcohol into all the raw materials weighed in the step 1, and stirring and grinding to obtain a suspension;
and step 3: standing the suspension obtained in the step 2 in air until the supernatant and the precipitate are obviously layered, and drying to obtain a mixed raw material;
and 4, step 4: pressing the mixed raw material obtained in the step 3 into a round sheet shape;
and 5: putting the wafer pressed in the step 4 into a high-temperature muffle furnace, heating to 1400-1500 ℃, sintering for 250-420 min, cooling to room temperature, taking out, and grinding to obtain powder, namely the fluorescent powder Ba 3 Eu 1-x RE x Al 2-y M y O 7.5 。
Further, the purity of each raw material in step 1 is more than 99.9%.
Further, in step 1, the raw material may be replaced with other replaceable materials, such as Al (OH) 3 Can be replaced by Al 2 O 3 。
Further, the container of the suspension in step 2 is an agate mortar or a glass beaker.
Further, in the step 2, the concentration of the suspension is 0.23-0.55 g of raw materials in each milliliter of anhydrous ethanol.
Further, the drying temperature in the step 3 is set to be 40-70 ℃ so as to avoid the deviation of components from a theoretical value caused by the boiling of absolute ethyl alcohol, the drying time is 5-8 hours, and the absolute ethyl alcohol is ensured to be completely evaporated.
Further, the pressing pressure in the step 4 is set to be 20-30 MPa, and the pressing pressure is maintained for 15-30 min to ensure that the mixed raw materials are fully compacted.
The invention has the beneficial effects that:
the fluorescence with negative thermal quenching behavior proposed by the inventionPowder Ba 3 Eu 1-x RE x Al 2-y M y O 7.5 The fluorescent material can emit strong orange red light under the excitation of UV/NUV light, has the characteristics of negative thermal quenching behavior that the luminescent color is stable and the luminescent intensity is gradually increased along with the increase of the temperature within 30-300 ℃, and has the advantages of simple process, high yield and high repeatability.
Drawings
FIG. 1 shows the phosphor Ba of the present invention 3 Eu 1-x RE x Al 2-y M y O 7.5 Powder X-ray diffraction spectrum contrast with standard cards;
FIG. 2 shows the phosphor Ba of the present invention 3 Eu 1-x RE x Al 2-y M y O 7.5 Excitation spectra at room temperature;
FIG. 3 shows a phosphor Ba of the present invention 3 Eu 1-x RE x Al 2-y M y O 7.5 An emission spectrum under the excitation of 272nm light at room temperature;
FIG. 4 shows a phosphor Ba of the present invention 3 Eu 1-x RE x Al 2-y M y O 7.5 An emission spectrum under room temperature and 391nm light excitation;
FIG. 5 shows phosphor Ba obtained in example 1 of the present invention 3 EuAl 1.99 Ga 0.01 O 7.5 An integral graph of the change of the luminous intensity with the temperature under the excitation of UV light (272nm) within 30-300 ℃;
FIG. 6 shows phosphor Ba obtained in example 1 of the present invention 3 EuAl 1.99 Ga 0.01 O 7.5 An integral graph of the change of the luminous intensity with the temperature under the excitation of NUV light (392nm) within 30-300 ℃;
FIG. 7 shows Ba phosphor obtained in example 2 of the present invention 3 Eu 0.99 Gd 0.01 Al 2 O 7.5 An integral graph of the change of the luminous intensity with the temperature under the excitation of UV light (272nm) within 30-300 ℃;
FIG. 8 shows phosphor Ba obtained in example 2 of the present invention 3 Eu 0.99 Gd 0.01 Al 2 O 7.5 An integral graph of the change of the luminous intensity with the temperature under the excitation of NUV light (392nm) within 30-300 ℃;
FIG. 9 shows phosphor Ba obtained in example 3 of the present invention 3 Eu 0.99 La 0.01 Al 2 O 7.5 An integral graph of the change of the luminous intensity with the temperature under the excitation of UV light (272nm) within 30-300 ℃;
FIG. 10 shows phosphor Ba obtained in example 3 of the present invention 3 Eu 0.99 La 0.01 Al 2 O 7.5 An integral graph of the change of the luminous intensity with the temperature under the excitation of NUV light (392nm) within 30-300 ℃.
Detailed Description
The technical means adopted by the invention are further described by combining the following specific embodiments.
Example 1
This example presents a phosphor Ba with negative thermal quenching behavior 3 EuAl 1.99 Ga 0.01 O 7.5 Belongs to a monoclinic system, and comprises the following specific preparation steps:
step 1: the raw material BaCO with the purity of more than 99.9 percent 3 、Eu 2 O 3 、Ga 2 O 3 、Al(OH) 3 Weighing 2.6049g of BaCO respectively according to molar ratio 3 0.7039g Eu 2 O 3 0.0037g of Ga 2 O 3 And 0.6209g of Al (OH) 3 ；
Step 2: putting all the raw materials weighed in the step 1 into an agate mortar, adding 30ml of absolute ethyl alcohol as a dispersion medium, fully grinding and uniformly mixing to obtain a suspension;
and 3, step 3: standing the suspension obtained in the step 2 for a period of time, putting the suspension into a drying oven, setting the drying temperature to be 60 ℃, and drying for 8 hours to completely evaporate the absolute ethyl alcohol to obtain a mixed raw material;
and 4, step 4: grinding the mixed raw material obtained in the step 3 again to enable the components to be mixed more uniformly, pressing the mixed raw material into a round sheet shape by using a powder tablet press, wherein the pressure is 30MPa, and maintaining for 15 min;
and 5: putting the wafer pressed in the step 4 into an alumina crucible, then putting the wafer into a high-temperature muffle furnace, heating to 1450 ℃, preserving the temperature for 300min to ensure that the raw materials are fully reacted, then cooling to room temperature along with the furnace, taking out the sample, and grinding to obtain Ba 3 EuAl 1.99 Ga 0.01 O 7.5 A powder material.
Example 2
This example presents a phosphor Ba with negative thermal quenching behavior 3 Eu 0.99 Gd 0.01 Al 2 O 7.5 Belongs to a monoclinic system, and comprises the following specific preparation steps:
step 1: the raw material BaCO with the purity of more than 99.9 percent 3 、Eu 2 O 3 、Gd 2 O 3 、Al(OH) 3 Weighing 2.6049g of BaCO respectively according to molar ratio 3 0.6968g of Eu 2 O 3 0.0073g of Gd 2 O 3 And 0.6240g of Al (OH) 3 ；
Step 2: putting all the raw materials weighed in the step 1 into an agate mortar, adding 30ml of absolute ethyl alcohol as a dispersion medium, fully grinding and uniformly mixing to obtain a suspension;
and step 3: standing the suspension obtained in the step 2 for a period of time, putting the suspension into a drying oven, setting the drying temperature to be 60 ℃, and drying for 8 hours to completely evaporate the absolute ethyl alcohol to obtain a mixed raw material;
and 4, step 4: grinding the mixed raw material obtained in the step 3 again to enable the components to be mixed more uniformly, pressing the mixed raw material into a round sheet shape by using a powder tablet press, wherein the pressure is 30MPa, and maintaining for 15 min;
and 5: putting the wafer pressed in the step 4 into an alumina crucible, then putting the wafer into a high-temperature muffle furnace, heating to 1500 ℃, preserving the temperature for 300min to ensure that the raw materials fully react, then cooling to room temperature along with the furnace, taking out the sample, and grinding to obtain Ba 3 Eu 0.99 Gd 0.01 Al 2 O 7.5 A powder material.
Example 3
This example presents phosphor B with negative thermal quenching behaviora 3 Eu 0.99 La 0.01 Al 2 O 7.5 Belongs to a monoclinic system, and comprises the following specific preparation steps:
step 1: the raw material BaCO with the purity of more than 99.9 percent 3 、Eu 2 O 3 、La 2 O 3 、Al(OH) 3 Weighing 2.6049g of BaCO respectively according to molar ratio 3 0.6968g of Eu 2 O 3 0.0065g of La 2 O 3 And 0.6240g of Al (OH) 3 ；
Step 2: putting all the raw materials weighed in the step 1 into an agate mortar, adding 30ml of absolute ethyl alcohol as a dispersion medium, fully grinding and uniformly mixing to obtain a suspension;
and step 3: standing the suspension obtained in the step 2 for a period of time, putting the suspension into a drying oven, setting the drying temperature to be 60 ℃, and drying for 8 hours to completely evaporate the absolute ethyl alcohol to obtain a mixed raw material;
and 4, step 4: grinding the mixed raw material obtained in the step 3 again to enable the components to be mixed more uniformly, pressing the mixed raw material into a round sheet shape by using a powder tablet press, wherein the pressure is 30MPa, and maintaining for 15 min;
and 5: putting the wafer pressed in the step 4 into an alumina crucible, then placing the wafer into a high-temperature muffle furnace, heating to 1500 ℃, preserving heat for 300min to ensure that the raw materials fully react, then cooling to room temperature along with the furnace, taking out a sample, and grinding to obtain Ba 3 Eu 0.99 La 0.01 Al 2 O 7.5 A powder material.
Example 4
This example presents a phosphor Ba with negative thermal quenching behavior 3 EuAl 1.98 Ga 0.02 O 7.5 Belongs to a monoclinic system, and comprises the following specific preparation steps:
step 1: the raw material BaCO with the purity of more than 99.9 percent 3 、Eu 2 O 3 、Ga 2 O 3 、Al(OH) 3 Weighing 2.6049g of BaCO respectively according to molar ratio 3 0.7039g Eu 2 O 3 0.0075g of Ga 2 O 3 And 0.6178g of Al (OH) 3 ；
Step 2: putting all the raw materials weighed in the step 1 into an agate mortar, adding 30ml of absolute ethyl alcohol as a dispersion medium, fully grinding and uniformly mixing to obtain a suspension;
and step 3: standing the suspension obtained in the step (2) for a period of time, putting the suspension into a drying box, setting the drying temperature to be 60 ℃, and drying for 8 hours to completely evaporate the anhydrous ethanol to obtain a mixed raw material;
and 4, step 4: grinding the mixed raw material obtained in the step 3 again to enable the components to be mixed more uniformly, and then pressing the mixed raw material into a round sheet shape by using a powder tablet press, wherein the pressure is 30MPa, and maintaining for 15 min;
and 5: putting the wafer pressed in the step 4 into an alumina crucible, then putting the wafer into a high-temperature muffle furnace, heating to 1500 ℃, preserving the temperature for 300min to ensure that the raw materials fully react, then cooling to room temperature along with the furnace, taking out the sample, and grinding to obtain Ba 3 EuAl 1.98 Ga 0.02 O 7.5 A powder material.
Example 5
This example presents a phosphor Ba with negative thermal quenching behavior 3 Eu 0.95 La 0.05 Al 2 O 7.5 Belongs to a monoclinic system, and comprises the following specific preparation steps:
step 1: the raw material BaCO with the purity of more than 99.9 percent 3 、Eu 2 O 3 、La 2 O 3 、Al(OH) 3 Weighing 2.6049g of BaCO respectively according to molar ratio 3 0.6687g Eu 2 O 3 0.0326g of La 2 O 3 And 0.6240g of Al (OH) 3 ；
Step 2: putting all the raw materials weighed in the step 1 into an agate mortar, adding 30ml of absolute ethyl alcohol as a dispersion medium, fully grinding and uniformly mixing to obtain a suspension;
and step 3: standing the suspension obtained in the step 2 for a period of time, putting the suspension into a drying oven, setting the drying temperature to be 60 ℃, and drying for 8 hours to completely evaporate the absolute ethyl alcohol to obtain a mixed raw material;
and 4, step 4: grinding the mixed raw material obtained in the step 3 again to enable the components to be mixed more uniformly, pressing the mixed raw material into a round sheet shape by using a powder tablet press, wherein the pressure is 30MPa, and maintaining for 15 min;
and 5: putting the wafer pressed in the step 4 into an alumina crucible, then putting the wafer into a high-temperature muffle furnace, heating to 1500 ℃, preserving the temperature for 300min to ensure that the raw materials fully react, then cooling to room temperature along with the furnace, taking out the sample, and grinding to obtain Ba 3 Eu 0.95 La 0.05 Al 2 O 7.5 A powder material.
Example 6
This example presents a phosphor Ba with negative thermal quenching behavior 3 Eu 0.95 Gd 0.05 Al 2 O 7.5 Belongs to a monoclinic system, and comprises the following specific preparation steps:
step 1: the raw material BaCO with the purity of more than 99.9 percent 3 、Eu 2 O 3 、Gd 2 O 3 、Al(OH) 3 Weighing 2.6049g of BaCO respectively according to molar ratio 3 0.6687g of Eu 2 O 3 0.0363g of Gd 2 O 3 And 0.6240g of Al (OH) 3 ；
Step 2: putting all the raw materials weighed in the step 1 into an agate mortar, adding 30ml of absolute ethyl alcohol as a dispersion medium, fully grinding and uniformly mixing to obtain a suspension;
and 3, step 3: standing the suspension obtained in the step 2 for a period of time, putting the suspension into a drying oven, setting the drying temperature to be 60 ℃, and drying for 8 hours to completely evaporate the absolute ethyl alcohol to obtain a mixed raw material;
and 4, step 4: grinding the mixed raw material obtained in the step 3 again to enable the components to be mixed more uniformly, and then pressing the mixed raw material into a round sheet shape by using a powder tablet press, wherein the pressure is 30MPa, and maintaining for 15 min;
and 5: putting the wafer pressed in the step 4 into an alumina crucible, then putting the wafer into a high-temperature muffle furnace, heating to 1500 ℃, preserving the temperature for 300min to ensure that the raw materials fully react, then cooling to room temperature along with the furnace, taking out the sample, and grinding to obtain Ba 3 Eu 0.95 Gd 0.05 Al 2 O 7.5 A powder material.
For the fluorescent powder Ba of the invention 3 Eu 1-x RE x Al 2-y M y O 7.5 When X is 0, Y is 0.01, M is Ga or Si, when Y is 0, X is 0.01, RE is La, Lu, Y or Gd, when Y is 0, X is 0.05, RE is La or Gd, and when X is 0, Y is 0.02, M is Ga, the powder material is subjected to an X-ray diffraction test, respectively, and compared with a phase having a PDF card number of 37-0291, as a result, as shown in fig. 1, it is known that the crystal structure of the powder material almost coincides with the phase having a PDF card number of 37-0291, and the crystal structure coincides with Ba card number of 37-0291 3 YAl 2 O 7.5 The material approximation indicates the successful preparation of monoclinic phase powder material.
For the fluorescent powder Ba of the invention 3 Eu 1-x RE x Al 2-y M y O 7.5 When x is 0, Y is 0.01, and M is Ga or Si, and when Y is 0, x is 0.01, and RE is one of La, Lu, Y, and Gd, as can be seen from the excitation spectrum at room temperature shown in fig. 2, the emission peak of the above-mentioned powder material with a monitoring center wavelength of 593nm can be excited by light of 272nm and 392 nm; as can be seen from the emission spectra at room temperature shown in FIGS. 3 and 4, the above-mentioned powder material can be excited by UV-NUV light with a wavelength of 272nm or 392nm and emits a strong orange-red light.
FIGS. 5 to 6 show the phosphors Ba obtained in example 1 3 EuAl 1.99 Ga 0.01 O 7.5 Under the excitation of UV light (272nm) and NUV light (392nm), the integral graphs of the change of the luminous intensity with the temperature within 30-300 ℃, and FIGS. 7-8 are respectively the Ba powder obtained in example 2 3 Eu 0.99 Gd 0.01 Al 2 O 7.5 Under the excitation of UV light (272nm) and NUV light (392nm), the integral graphs of the luminous intensity with the temperature change within 30-300 ℃, and figures 9-10 are the Ba phosphor powder obtained in example 3 respectively 3 Eu 0.99 La 0.01 Al 2 O 7.5 The integral graph of the change of the emission intensity with temperature at 30-300 ℃ under the excitation of UV light (272nm) and NUV light (392nm) shows that the powder materials obtained in examples 1-3 are excited by UV (270nm)/NUV (392nm),the material shows negative thermal quenching behavior at 30-300 ℃. Especially under 392nm excitation, the emission intensity can increase to around 1.7 times the initial temperature when the temperature is raised to 300 ℃.
Claims (7)
1. Fluorescent powder Ba with negative thermal quenching behavior 3 Eu 1-x RE x Al 2-y M y O 7.5 Characterized in that it belongs to the monoclinic system, space group is P2/c, unit cell parameters are
Wherein RE is one of La, Lu, Y and Gd, and M is Ga or Si; when x is 0, y is 0.01-0.02; when y is 0, x is 0.01 to 0.05.
2. The phosphor Ba of claim 1, having negative thermal quenching behavior 3 Eu 1-x RE x Al 2-y M y O 7.5 Characterized in that the phosphor powder Ba 3 Eu 1-x RE x Al 2-y M y O 7.5 Under the excitation of UV-NUV light, the material has negative thermal quenching behavior at the temperature of 30-300 ℃.
3. Fluorescent powder Ba with negative thermal quenching behavior 3 Eu 1-x RE x Al 2-y M y O 7.5 The preparation method is characterized by comprising the following steps:
step 1: according to the mole ratio of elements Ba, Eu, RE, Al and M being 3: (1-x): x: (2-y): weighing the raw material BaCO according to the proportion of y 3 、Eu 2 O 3 、RE 2 O 3 、Al(OH) 3 And M 2 O 3 (ii) a Wherein RE is one of La, Lu, Y and Gd, and M is Ga or Si; when x is 0, y is 0.01-0.02; when y is 0, x is 0.01-0.05;
step 2: adding absolute ethyl alcohol into all the raw materials in the step 1, and stirring and grinding to obtain a suspension;
and step 3: standing the suspension in air until the supernatant and the precipitate are obviously layered, and drying to obtain a mixed raw material;
and 4, step 4: pressing the mixed raw materials into a round sheet shape;
and 5: putting the wafer pressed in the step 4 into a high-temperature muffle furnace, heating to 1400-1500 ℃, sintering for 250-420 min, cooling to room temperature, taking out, and grinding to obtain powder, namely the fluorescent powder Ba 3 Eu 1-x RE x Al 2-y M y O 7.5 。
4. The phosphor Ba of claim 3 having negative thermal quenching behavior 3 Eu 1-x RE x Al 2-y M y O 7.5 The production method of (1) is characterized in that Al (OH) 3 Substitution by Al 2 O 3 。
5. The phosphor Ba of claim 3 having negative thermal quenching behavior 3 Eu 1-x RE x Al 2-y M y O 7.5 The preparation method is characterized in that in the step 2, the concentration of the suspension is 0.23-0.55 g of raw materials in each milliliter of absolute ethyl alcohol.
6. The phosphor Ba of claim 3 having negative thermal quenching behavior 3 Eu 1-x RE x Al 2-y M y O 7.5 The preparation method is characterized in that in the step 3, the drying temperature is 40-70 ℃, and the drying time is 5-8 hours.
7. The phosphor Ba of claim 3 having negative thermal quenching behavior 3 Eu 1-x RE x Al 2-y M y O 7.5 The preparation method is characterized in that in the step 4, the pressing pressure is 20-30 MPa and is maintained for 15-30 min.
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| JP2015221843A (en) * | 2014-05-22 | 2015-12-10 | パナソニック株式会社 | Fluophor and light-emitting device using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102492425A (en) * | 2011-11-24 | 2012-06-13 | 苏州大学 | Aluminate red phosphor, preparation method and application |
| JP2015137328A (en) * | 2014-01-23 | 2015-07-30 | 国立大学法人 新潟大学 | Ce3+ ACTIVATED OXIDE PHOSPHOR |
| JP2015221843A (en) * | 2014-05-22 | 2015-12-10 | パナソニック株式会社 | Fluophor and light-emitting device using the same |
| CN113897197A (en) * | 2021-10-25 | 2022-01-07 | 大连民族大学 | High-thermal-stability blue light emitting fluorescent material and preparation method and application thereof |
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| ANNA C. DUKE ET AL.: "Yellow-green luminescence and extreme thermal quenching in the Sr6M2Al4O15:Eu2+ (M = Y, Lu, Sc) phosphor series" * |
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