CN111909697A - White long-afterglow luminescent material and preparation method thereof - Google Patents

White long-afterglow luminescent material and preparation method thereof Download PDF

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CN111909697A
CN111909697A CN202010921313.6A CN202010921313A CN111909697A CN 111909697 A CN111909697 A CN 111909697A CN 202010921313 A CN202010921313 A CN 202010921313A CN 111909697 A CN111909697 A CN 111909697A
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grinding
afterglow
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CN111909697B (en
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陈文波
严娟
梁国昌
冉红梅
聂明航
张辉
夏继宏
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Chongqing University of Arts and Sciences
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Abstract

A white long-afterglow luminescent material is characterized in that: the molecular formula is Ca5‑xGa6O14:Pr3+ xWherein, Pr3+As an activator, Ca5‑xGa6O14Is matrix, x is more than or equal to 0.005 and less than or equal to 0.09. The white long afterglow luminescent material has high purity, homogeneous shape, homogeneous size distribution, high light color purity, about 10 micron, white afterglow after being excited by several excitation sources, and initial brightness of 0.7766cd/m after being excited by 254nm wavelength ultraviolet light for 5min2The maximum afterglow time can reach more than 13 hours, and the afterglow brightness can still be kept at 10mcd/m when the afterglow time reaches 10 hours2The above.

Description

White long-afterglow luminescent material and preparation method thereof
Technical Field
The invention relates to the technical field of luminescent materials, in particular to a white long-afterglow luminescent material and a preparation method thereof.
Background
The afterglow luminescent material is an important optical functional material. It is known that it absorbs and stores energy under the irradiation of sunlight, fluorescent or incandescent lamps, etc., and then emits visible or near-infrared light within minutes or tens of minutes after the excitation light source is removed. Generally, it relies on the release of carriers trapped in traps after the excitation is stopped. The light-emitting diode can release the captured carriers under the action of heat energy at room temperature, so that durable light emission is generated. Over the past decades, persistent luminescent materials have gained explosive development due to their widespread use, such as emergency escape signs, optical information storage and road markings visible in the dark. Since the green and blue long afterglow materials reach the commercial requirement, people try to develop the red long afterglow material so as to realize the long afterglow materials with different colors by mixing three primary colors, thereby meeting various application requirements. In fact, it is difficult to realize long-afterglow luminescent materials of other colors by a three-primary color mixing method because the substrates of the long-afterglow luminescent materials of three primary colors are different, and each component has different chemical, physical and thermal properties after mixing the different luminescent materials. Due to these differences in properties, consistency cannot be maintained during afterglow decay, making it difficult to control the balance of color ratios. Although the method overcomes the problem that the long afterglow materials prepared by mixing three primary colors cannot be excited by the same wavelength and have inconsistent attenuation of different colors, the afterglow of the afterglow materials is shorter, the afterglow brightness is low and the afterglow stability is poor.
In previous studies, Pr has been demonstrated3+The ions may emit a variety of colors. At present there is little concern about Pr3+The report of ion white LPL fluorescent powder needs proper crystal field condition to control the control ratio of blue-green color and red color, so that it can implement white long afterglow property material on single substrate, and in the actual preparation process, the crystal field condition is difficult to control, and other substrates are easy to produce in the preparation process, and when the materials are doped, the reaction is easy to be incomplete, and several kinds of materials can be producedImpurities and Pr3+The prepared material is difficult to be doped into a matrix, the agglomeration is serious, the size span is large, the afterglow color emitted by the material is affected to be impure, the afterglow emitted after excitation has other colors, the afterglow brightness is low, the afterglow is attenuated violently, and the afterglow duration is short.
Disclosure of Invention
Based on the technical problems, the invention aims to provide a white long-afterglow luminescent material. The material is multi-excitation source luminous, and has high afterglow brightness and long afterglow duration.
The invention also aims to provide a preparation method of the white long-afterglow luminescent material.
The purpose of the invention is realized by the following technical scheme:
a white long-afterglow luminescent material is characterized in that: the molecular formula is Ca5-xGa6O14: Pr3+ xWherein, Pr3+As an activator, Ca5-xGa6O14Is matrix, x is more than or equal to 0.005 and less than or equal to 0.09.
Further, the white long afterglow luminescent material is CaCO3、Ga2O3、 Pr6O11The material is prepared by grinding and drying the raw materials in sequence to prepare raw material powder, and then calcining, grinding and calcining the raw material powder.
The preparation method of the white long-afterglow luminescent material is characterized by comprising the following steps: grinding and drying are sequentially carried out to prepare raw material powder, and then composite calcination including primary calcination, grinding and secondary calcination is carried out, wherein the primary composite calcination is to place the raw material powder in an air environment at 1210-1280 ℃ for sintering for 6-9 h, the sintering is carried out after the temperature is reduced to the room temperature, the grinding is carried out, and the secondary calcination is to sinter the raw material powder in a reducing atmosphere at 900-1000 ℃ for 2-4 h and cool the sintering to the room temperature.
Preferably, the first calcination is carried out at 1250 ℃ for 8 hours, and the second calcination is carried out at 1000 ℃ for 3 hours.
Further, the reducing atmosphere is composed of 10% by volume of H2And 90% by volume of N2And (4) forming.
Furthermore, the grinding in the composite calcination is carried out from inside to outside along the same direction, the grinding speed is 40 r/min, and the grinding time exceeds 15 min.
Preferably, the grinding time is 20 to 40 min.
Further, CaCO produced from the above raw material powder3、Ga2O3、 Pr6O11Adding absolute ethyl alcohol as a raw material, and grinding at the temperature lower than 20 ℃, wherein the grinding speed is 30 revolutions per minute, and the grinding time is 45-70 min.
Further, the above-mentioned CaCO3、Ga2O3、Pr6O11The mass ratio of (A) to (B) is 0.589-0.599: 0.667: 0.001-0.182.
Further, the use amount of the absolute ethyl alcohol and the total mass of the raw materials is 1-1.2: 1.
further, the above drying is to dry the ground powder at 100 ℃ for 2 hours.
Most particularly, the preparation method of the white long-afterglow luminescent material is characterized by comprising the following steps:
(1) preparation of the starting powder
According to CaCO3、Ga2O3、 Pr6O11The mass ratio of CaCO to the total amount of the CaCO is 0.589-0.599: 0.667: 0.001-0.1823、Ga2O3、 Pr6O11Adding absolute ethyl alcohol as a raw material, wherein the mass ratio of the absolute ethyl alcohol to the total mass of the raw material is 1-1.2: 1, grinding at the temperature lower than 20 ℃, wherein the grinding speed is 30 r/min, and drying the powder at the temperature of 100 ℃ for 2h after grinding;
(2) composite calcination
The first calcination is to place the raw material powder in an air environment with the temperature of 1210-1280 ℃, sinter the raw material powder for 6-8 hours, cool the raw material powder to room temperature, grind the raw material powder from inside to outside along the same direction, wherein the grinding speed is 40 r/min, the grinding time is more than 15min, and then the raw material powder is ground by H with the volume percentage of 10 percent2And 90% by volume of N2And (3) calcining for the second time in the reducing atmosphere of the composition at the temperature of 900-1000 ℃, sintering for 2-4 h, and cooling to room temperature.
In the process of calcination, Pr3+Difficult to dope into the matrix, and the presence of CaGa in the product obtained during calcination2O4，Ca3Ga4O9Or CaGa4O7CaO and Ga may also be present2O3And the product has poor dispersibility due to impurities, large aggregates are formed, the size difference among particles is large, and the particles are distributed in the range of 0.5-300 mu m. The invention passes through CaCO with specific mass proportion3、Ga2O3、 Pr6O11Preparing raw material powder by a specific grinding means, improving the dispersibility of the raw material powder, combining with first high-temperature calcination, then performing specific grinding and low-temperature reduction to ensure full and complete reaction, and Pr3+Effectively doped into the matrix and substituted, thereby reducing the agglomeration degree of crystals and reducing the generation of impurities, and finally obtaining the Ca with good dispersibility, uniform size distribution and high purity5-xGa6O14: Pr3+ xThe material is a white long-afterglow luminescent material with high photochromic purity.
The invention has the following technical effects:
the white long afterglow luminescent material has high purity, homogeneous shape, homogeneous size distribution, high light color purity, about 10 micron, white afterglow after being excited by several excitation sources, and initial brightness of 0.7766cd/m after being excited by 254nm wavelength ultraviolet light for 5min2The maximum afterglow time can reach more than 13 hours, and the afterglow brightness can still be kept at 50mcd/m when the afterglow time reaches 10 hours2The above.
The method for preparing the white long-afterglow luminescent material ensures that the product has high purity, good dispersibility, uniform appearance and uniform size which is about 10 mu m, and the initial brightness of white afterglow reaches 0.7766cd/m after being excited by ultraviolet light with the wavelength of 254nm for 5 minutes2The maximum time can reach more than 13 hours, and the afterglow brightness still keeps 50mcd/m when the afterglow time reaches 10 hours2As described above, the composition has excellent afterglow performance stability.
Drawings
FIG. 1: the X-ray powder diffraction of the long afterglow material prepared by the invention is compared with the standard card 78-1180.
FIG. 2: scanning electron microscope images of the white long afterglow luminescent materials prepared in the embodiment 1 of the present invention.
FIG. 3: the afterglow spectrum of the white long afterglow luminescent material prepared in the embodiment 1 of the invention is excited by 254nm ultraviolet light for 5 min.
FIG. 4: the afterglow spectrum of the white long afterglow luminescent material prepared in the embodiment 1 of the invention after being excited by X-ray for 60 s.
FIG. 5: the afterglow decay curve graph of the white long afterglow luminescent material prepared in the embodiment 1 of the invention after being excited by 254nm ultraviolet light for 5 min.
Detailed Description
The present invention is described in detail below by way of examples, it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and those skilled in the art can make some insubstantial modifications and adaptations of the present invention based on the above-mentioned disclosure.
Example 1
White long-afterglow luminescent material Ca4.93Ga6O14:Pr0.07 3+The preparation method comprises the following steps:
(1) preparation of the starting powder
According to 0.5915gCaCO3、0.6673gGa2O3And 0.0141g Pr6O11Mixing the raw materials, adding absolute ethyl alcohol, wherein the mass ratio of the absolute ethyl alcohol to the total mass of the raw materials is 1: 1, grinding at the temperature lower than 15 ℃, wherein the grinding speed is 30 revolutions per minute, the grinding time is 50 minutes, and after grinding, drying the powder at the temperature of 100 ℃ for 2 hours;
(2) composite calcination
Placing the raw material powder prepared in the step (1) in an air environment at 1250 ℃, sintering for 8H, cooling to room temperature, grinding from inside to outside along the same direction, wherein the grinding speed is 40 revolutions per minute, the grinding time is 25min, and then grinding with H with the volume percentage of 10%2And 90 volume percent% of N2And (3) calcining for the second time in the reducing atmosphere of the composition at the temperature of 1000 ℃, sintering for 3 hours, and cooling to room temperature.
The comparison graph of X-ray diffraction of the white long afterglow luminescent material prepared in the embodiment and the standard card 78-1180 is shown in FIG. 1, and the comparison with the standard card shows that the peak can be well matched, no impurity peak appears, and the description shows that Pr is good3+The matrix structure is not changed by adding (2), and the sample can be judged to be a single phase.
As shown in figure 2, a scanning electron microscope of the long afterglow material can clearly observe a white particle sample of about 10 microns, and the sample is uniformly distributed and has low agglomeration degree.
As shown in FIG. 3, the afterglow spectrum of the long afterglow luminescent material excited by ultraviolet light having a wavelength of 254nm has been related to Pr3+Reports of doped luminescent materials have focused mainly on1D2At a dominant transition, most of which are from3P0→3H4Showing a weak transition. But discovered in later related studies to3P0→3H4Dominant emission may be achieved. The long afterglow spectrum of the material contains3P0And1D2multiple electron at Pr3+The 4f energy level transition of the light source generates green-blue and red components, and the different colors emit the expected white long afterglow after being mixed in a certain ratio. The color coordinates of the long-afterglow luminescent material afterglow calculated by using a CIE chromaticity diagram are x =0.3203 and y =0.3385, and the long-afterglow luminescent material afterglow is positioned in a white light emitting area. The prepared long-afterglow luminescent material can be indicated as a white long-afterglow luminescent material.
The afterglow decay curve of the white long afterglow luminescent material after being excited by X-ray for 60 seconds is shown in figure 4, and it can be found that the peak shape and the peak position of the afterglow spectrum are consistent with the afterglow spectrum excited by an ultraviolet lamp, and the afterglow mechanism is also consistent. We also try to use other wave band light sources such as blue light of about 480nm and yellow light of 530-630nm to respectively excite the long afterglow material prepared by the invention, and the long afterglow material can generate white afterglow after excitation, the afterglow spectrum is basically consistent with the afterglow spectrum excited by ultraviolet light, and the afterglow time can reach more than 10 hours. Therefore, the white long-afterglow luminescent material prepared by the invention is determined to be a long-afterglow luminescent material with multiple excitation sources.
The afterglow decay curve of the long afterglow material after being excited by ultraviolet light with the wavelength of 254nm for 5min is shown in figure 5, and the initial afterglow brightness of the long afterglow material reaches 0.7766cd/m2The luminance of the sample is shown as a function of time. The lowest luminance observable by human eyes is 0.32mcd/m2And the white afterglow emitted by the long afterglow material can be kept above the brightness for more than 13.6 hours. As can be seen from the figure, in the present embodiment, in the initial stage of the long afterglow phosphor, the afterglow decays rapidly and slowly to a certain value, and the afterglow luminance is still maintained at 90mcd/m when the afterglow duration reaches 10h2As described above, the afterglow stability during the attenuation process is excellent, indicating that the afterglow performance is excellent.
Example 2
White long-afterglow luminescent material Ca4.91Ga6O14:Pr0.09 3+The preparation method comprises the following steps:
(1) preparation of the starting powder
Weighing 0.5891gCaCO3、0.6673gGa2O3And 0.0182g Pr6O11Adding absolute ethyl alcohol as a raw material, wherein the mass ratio of the absolute ethyl alcohol to the total mass of the raw material is 1.1: 1, grinding at 10 ℃, wherein the grinding speed is 30 r/min, the grinding time is 45min, and after grinding, drying the powder at 100 ℃ for 2 h;
(2) composite calcination
The first calcination is to place the raw material powder in an air environment at 1280 ℃, sinter the raw material powder for 6 hours, cool the raw material powder to room temperature, grind the raw material powder from inside to outside along the same direction, wherein the grinding speed is 40 r/min, the grinding time is 30min, and then the raw material powder is ground by H with the volume percentage of 10 percent2And 90% by volume of N2And (3) calcining for the second time in the reducing atmosphere of the composition at 950 ℃, sintering for 2 hours, and cooling to room temperature.
The white cake prepared in this exampleGlow material Ca4.91Ga6O14:Pr0.09 3+Excellent dispersivity and uniform size, the initial brightness of the white afterglow reaches 0.7600cd/m after being excited by ultraviolet light with the wavelength of 254nm for 5min2. The long afterglow material can maintain the white afterglow over the lowest brightness for human eye to over 13.2 hr. When the persistence time reaches 10h, the persistence brightness still reaches 67.8mcd/m2And the afterglow stability in the attenuation process is excellent.
Example 3
White long-afterglow luminescent material Ca4.995Ga6O14:Pr0.005 3+The preparation method comprises the following steps:
(1) preparation of the starting powder
Weighing 0.5992gCaCO3、0.6673gGa2O3And 0.001g Pr6O11Adding absolute ethyl alcohol as a raw material, wherein the mass ratio of the absolute ethyl alcohol to the total mass of the raw material is 1.2: 1, grinding at 20 ℃, wherein the grinding speed is 30 r/min, and drying the powder at 100 ℃ for 2h after grinding;
(2) composite calcination
The first calcination is to place the raw material powder in an air environment with 1210 ℃, sinter the raw material powder for 7H, cool the raw material powder to room temperature, grind the raw material powder from inside to outside along the same direction, wherein the grinding speed is 40 r/min, the grinding time is 15min, and then grind the raw material powder in H with the volume percentage of 10 percent2And 90% by volume of N2And (3) calcining for the second time in the reducing atmosphere of the composition at the temperature of 900 ℃, sintering for 4 hours, and cooling to room temperature.
The white long-afterglow luminescent material Ca prepared in this example4.995Ga6O14:Pr0.005 3+After being excited by ultraviolet light with the wavelength of 254nm for 5min, the initial brightness of the white afterglow emitted by the long afterglow material reaches 0.7570cd/m2. The afterglow of the long afterglow material can be maintained above the lowest brightness observable by human eyes for more than 13.7 hours. When the persistence time reaches 10h, the persistence brightness stillReaches 79.3mcd/m2And the afterglow stability in the attenuation process is excellent.
Example 4
White long-afterglow luminescent material Ca4.93Ga6O14:Pr0.07 3+The preparation method comprises the following steps:
(1) preparation of the starting powder
According to 0.5915gCaCO3、0.6673gGa2O3And 0.0141g Pr6O11Mixing the raw materials, adding absolute ethyl alcohol, wherein the mass ratio of the absolute ethyl alcohol to the total mass of the raw materials is 1: 1, grinding at 15 ℃, wherein the grinding speed is 30 revolutions per minute, the grinding time is 60 minutes, and after grinding, drying the powder at 100 ℃ for 2 hours;
(2) composite calcination
Placing the raw material powder prepared in the step (1) in an air environment at 1250 ℃, sintering for 8H, cooling to room temperature, grinding from inside to outside along the same direction, wherein the grinding speed is 40 revolutions per minute, the grinding time is 25min, and then grinding with H with the volume percentage of 10%2And 90% by volume of N2And (3) calcining for the second time in the reducing atmosphere of the composition at the temperature of 1000 ℃, sintering for 3 hours, and cooling to room temperature.
The white long-afterglow luminescent material Ca prepared in this example4.93Ga6O14:Pr0.07 3+Excellent dispersivity and uniform size, the initial brightness of the white afterglow emitted by the long afterglow material reaches 0.7844cd/m after being excited by ultraviolet light with the wavelength of 254nm for 5min2. The afterglow of the long afterglow material can be maintained above the lowest brightness observable by human eyes for more than 13.4 hours. When the persistence time reaches 10h, the persistence brightness still reaches 64.6mcd/m2And the afterglow stability in the attenuation process is excellent.
Example 5
White long-afterglow luminescent material Ca4.99Ga6O14:Pr0.01 3+The preparation method comprises the following steps:
(1) preparation of the starting powder
According to 0.5986gCaCO3、0.6673gGa2O3And 0.002g Pr6O11Mixing the raw materials, adding absolute ethyl alcohol, wherein the mass ratio of the absolute ethyl alcohol to the total mass of the raw materials is 1: 1, grinding at 15 ℃, wherein the grinding speed is 30 r/min, the grinding time is 55min, and after grinding, drying the powder at 100 ℃ for 2 h;
(2) composite calcination
Placing the raw material powder prepared in the step (1) in an air environment at 1250 ℃, sintering for 8H, cooling to room temperature, grinding from inside to outside along the same direction, wherein the grinding speed is 40 revolutions per minute, the grinding time is 25min, and then grinding with H with the volume percentage of 10%2And 90% by volume of N2And (3) calcining for the second time in the reducing atmosphere of the composition at the temperature of 1000 ℃, sintering for 3 hours, and cooling to room temperature.
The white long-afterglow luminescent material Ca prepared in this example4.99Ga6O14:Pr0.01 3+Excellent dispersivity and uniform size, the initial brightness of the white afterglow reaches 0.7264cd/m after being excited by ultraviolet light with the wavelength of 254nm for 5min2. The long afterglow emitted by the long afterglow material can be kept above the lowest brightness which can be observed by human eyes for more than 13.05 hours. When the persistence time reaches 10h, the persistence brightness still reaches 53.7mcd/m2And the afterglow stability in the attenuation process is excellent.
Example 6
White long-afterglow luminescent material Ca4.95Ga6O14:Pr0.05 3+The preparation method comprises the following steps:
(1) preparation of the starting powder
According to 0.5939gCaCO3、0.6673gGa2O3And 0.01g Pr6O11Mixing the raw materials, adding absolute ethyl alcohol, wherein the mass ratio of the absolute ethyl alcohol to the total mass of the raw materials is 1: grinding at a temperature below 15 deg.C at a speed of 30 rpm for 70min, and subjecting the powder to 100 deg.CDrying for 2 hours;
(2) composite calcination
Placing the raw material powder prepared in the step (1) in an air environment at 1250 ℃, sintering for 8H, cooling to room temperature, grinding from inside to outside along the same direction, wherein the grinding speed is 40 revolutions per minute, the grinding time is 25min, and then grinding with H with the volume percentage of 10%2And 90% by volume of N2And (3) calcining for the second time in the reducing atmosphere of the composition at the temperature of 1000 ℃, sintering for 3 hours, and cooling to room temperature.
The white long-afterglow luminescent material Ca prepared in this example4.95Ga6O14:Pr0.05 3+Excellent dispersivity and uniform size, the initial brightness of the white afterglow emitted by the long afterglow material reaches 0.7558cd/m after being excited by ultraviolet light with the wavelength of 254nm for 5min2. The afterglow of the long afterglow material can be maintained above the lowest brightness observable by human eyes for more than 13.2 hours. When the persistence time reaches 10h, the persistence brightness still reaches 62.9mcd/m2And the afterglow stability in the attenuation process is excellent.

Claims (9)

1. A white long-afterglow luminescent material is characterized in that: the molecular formula is Ca5-xGa6O14: Pr3+ xWherein, Pr3+As an activator, Ca5-xGa6O14Is matrix, x is more than or equal to 0.005 and less than or equal to 0.09.
2. The white long-afterglow luminescent material of claim 1, wherein: the white long afterglow luminescent material is CaCO3、Ga2O3、 Pr6O11The material is prepared by grinding and drying the raw materials in sequence to prepare raw material powder, and then calcining, grinding and calcining the raw material powder.
3. The method for preparing a white long-afterglow luminescent material as claimed in claim 1 or 2, wherein: with CaCO3、Ga2O3、 Pr6O11Grinding and drying the raw materials in sequence to prepare raw material powder, and performing composite calcination including primary calcination, grinding and secondary calcination, wherein the primary composite calcination is to place the raw material powder in an air environment at 1210-1280 ℃ for sintering for 6-9 h, cool the raw material powder to room temperature, grind the raw material powder, and the secondary calcination is to sinter the raw material powder in a reducing atmosphere at 900-1000 ℃ for 2-4 h and cool the raw material powder to room temperature.
4. The method for preparing a white long-afterglow luminescent material as claimed in claim 3, wherein: the reducing atmosphere is composed of 10% by volume of H2And 90% by volume of N2And (4) forming.
5. The method for preparing a white long-afterglow luminescent material as claimed in claim 3 or 4, wherein: the grinding in the composite calcination is carried out from inside to outside along the same direction, the grinding speed is 40 r/min, and the grinding time is more than 15 min.
6. The method for preparing a white long-afterglow luminescent material as claimed in claim 3, wherein: in the process of preparing the raw material powder, absolute ethyl alcohol is added during grinding, and grinding is carried out at the temperature lower than 20 ℃, wherein the grinding speed is 30 revolutions per minute, and the grinding time is 45-70 minutes.
7. The method for preparing a white long-afterglow luminescent material as claimed in claim 5, wherein: the above CaCO3、Ga2O3、 Pr6O11The mass ratio of (A) to (B) is 0.589-0.599: 0.667: 0.001-0.182.
8. The method for preparing a white long-afterglow luminescent material as claimed in claim 6, wherein: the use amount of the absolute ethyl alcohol and the total mass of the raw materials is 1-1.2: 1.
9. a preparation method of a white long-afterglow luminescent material is characterized by comprising the following steps:
(1) preparation of the starting powder
According to CaCO3、Ga2O3、 Pr6O11The mass ratio of CaCO to the total amount of the CaCO is 0.589-0.599: 0.667: 0.001-0.1823、Ga2O3、 Pr6O11Adding absolute ethyl alcohol as a raw material, wherein the mass ratio of the absolute ethyl alcohol to the total mass of the raw material is 1-1.2: 1, grinding at the temperature lower than 20 ℃, wherein the grinding speed is 30 r/min, and drying the powder at the temperature of 100 ℃ for 2h after grinding;
(2) composite calcination
The first calcination is to place the raw material powder in an air environment with the temperature of 1210-1280 ℃, sinter the raw material powder for 6-8 hours, cool the raw material powder to room temperature, grind the raw material powder from inside to outside along the same direction, wherein the grinding speed is 40 r/min, the grinding time is more than 15min, and then the raw material powder is ground by H with the volume percentage of 10 percent2And 90% by volume of N2And (3) calcining for the second time in the reducing atmosphere of the composition at the temperature of 900-1000 ℃, sintering for 2-4 h, and cooling to room temperature.
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CN116554866A (en) * 2023-04-26 2023-08-08 桂林电子科技大学 Red stress luminescent fluorescent powder and preparation method thereof

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