CN111635757B - Preparation method of yellow-green long afterglow fluorescent material and application of ammonium bicarbonate - Google Patents
Preparation method of yellow-green long afterglow fluorescent material and application of ammonium bicarbonate Download PDFInfo
- Publication number
- CN111635757B CN111635757B CN202010496461.8A CN202010496461A CN111635757B CN 111635757 B CN111635757 B CN 111635757B CN 202010496461 A CN202010496461 A CN 202010496461A CN 111635757 B CN111635757 B CN 111635757B
- Authority
- CN
- China
- Prior art keywords
- yellow
- fluorescent material
- green long
- afterglow fluorescent
- raw material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7792—Aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/166—Strontium aluminates
Abstract
The invention discloses a preparation method of a yellow-green long afterglow fluorescent material. Uniformly mixing the raw material obtained according to the composition of the yellow-green long afterglow fluorescent material, the fluxing agent and the ammonium bicarbonate to obtain a mixture; calcining the mixture in a reducing atmosphere, and cooling a calcined product to obtain a yellow-green long afterglow fluorescent material; the yellow-green long afterglow fluorescent material comprises the following components: sr1‑x‑ yAl2O4:Eu2+ x,Dy3+ y. The preparation method can improve the luminous intensity of the yellow-green long-afterglow fluorescent material and reduce the afterglow decay rate. The invention also discloses the application of the ammonium bicarbonate in improving the luminous intensity of the yellow-green long-afterglow fluorescent material or reducing the afterglow decay rate of the yellow-green long-afterglow fluorescent material.
Description
Technical Field
The invention relates to a preparation method of a yellow-green long-afterglow fluorescent material and application of ammonium bicarbonate.
Background
The long afterglow fluorescent material is a photoluminescent material, can emit visible light and store energy after absorbing natural light or an illumination light source, and slowly releases the stored energy in the form of light after stopping the illumination of the light source to realize electroless luminescence, so the long afterglow fluorescent material is also called as a noctilucent material. At present, the long afterglow fluorescent material mainly takes aluminate, phosphate, sulfide and silicate as substrates. Among the long persistence fluorescent materials using these substances as the matrix, the aluminate-based fluorescent materials have the characteristics of high luminous efficiency and good chemical stability, and have been paid attention to.
SrAl developed in 90 s of 20 th century2O4:Eu2+,Dy3+The yellow-green long afterglow fluorescent material has high luminous intensity, high chemical stability and low costLow afterglow attenuation speed is long, and the advantages of no toxicity and no pollution are achieved, so that the method is widely applied to daily life, disaster prevention, military, fire fighting and the like. However, srAl2O4:Eu2+,Dy3+The luminous intensity of the yellow-green long afterglow fluorescent material and the reduction of the afterglow decay rate still need to be further improved.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a yellow-green long-afterglow fluorescent material, which can improve the luminous intensity of the yellow-green long-afterglow fluorescent material and reduce the afterglow decay rate.
On the other hand, the invention provides the application of the ammonium bicarbonate in improving the luminous intensity of the yellow-green long-afterglow fluorescent material and/or reducing the afterglow decay rate of the yellow-green long-afterglow fluorescent material.
The invention provides a preparation method of a yellow-green long afterglow fluorescent material, which comprises the following steps:
(1) Uniformly mixing the raw material obtained according to the composition of the yellowish green long-afterglow fluorescent material, a fluxing agent and ammonium bicarbonate to obtain a mixture;
(2) Calcining the mixture in a reducing atmosphere, and cooling a calcined product to obtain a yellow-green long afterglow fluorescent material;
wherein, the yellow-green long afterglow fluorescent material has the composition shown in formula (1):
Sr1-x-yAl2O4:Eu2+ x,Dy3+ y (1)
wherein x and y each represent Eu2+And Dy3+In a molar ratio of 0<x<1，0<y<1, and x + y<1。
The invention unexpectedly discovers that the ammonium bicarbonate is beneficial to improving the luminous intensity of the yellow-green long afterglow fluorescent material and reducing the afterglow decay rate.
According to the preparation method of the present invention, preferably, the ammonium bicarbonate is used in an amount of 3 to 80wt% based on the raw material. More preferably, the amount of ammonium bicarbonate is 40 to 60wt% of the starting material. According to one embodiment of the invention, the amount of ammonium bicarbonate is 50wt% of the starting material. Thus being beneficial to improving the luminous intensity of the yellow-green long afterglow fluorescent material and reducing the afterglow decay rate.
Preferably, 0.001< > x < -0.2,0.001 < > y < -0.1 in the production method according to the invention. More preferably, 0.001 woven-over x-woven-over 0.008,0.001 woven-over y-woven-over 0.008. Thus being beneficial to improving the luminous intensity of the yellow-green long afterglow fluorescent material.
In the present invention, the raw material of Sr element may be selected from one or more of strontium carbonate, strontium oxide, strontium oxalate, strontium hydroxide, and strontium sulfate. Examples of strontium carbonates include, but are not limited to, strontium carbonate. Examples of strontium oxides include, but are not limited to, strontium oxide. Examples of strontium oxalates include, but are not limited to, strontium oxalate. Examples of strontium hydroxide include, but are not limited to, strontium hydroxide. Examples of sulfates of strontium include, but are not limited to, strontium sulfate.
In the present invention, the raw material of Al element may be one or more selected from carbonate of aluminum, oxide of aluminum, oxalate of aluminum, hydroxide of aluminum, and sulfate of aluminum. Examples of aluminum carbonates include, but are not limited to, aluminum carbonate. Examples of oxides of aluminum include, but are not limited to, aluminum oxide. Examples of aluminum oxalates include, but are not limited to, aluminum oxalate. Examples of hydroxides of aluminum include, but are not limited to, aluminum hydroxide. Examples of aluminum sulfates include, but are not limited to, aluminum sulfate.
In the present invention, the raw material of Eu element may be selected from one or more of carbonate of europium, oxide of europium, oxalate of europium, hydroxide of europium, and sulfate of europium. Examples of europium carbonates include, but are not limited to, europium carbonate. Examples of oxides of europium include, but are not limited to, europium oxide. Examples of europium oxalates include, but are not limited to, europium oxalate. Examples of europium hydroxides include, but are not limited to, europium hydroxide. Examples of europium sulfates include, but are not limited to, europium sulfate.
In the present invention, the raw material of Dy element may be one or more selected from carbonate of dysprosium, oxide of dysprosium, oxalate of dysprosium, hydroxide of dysprosium, and sulfate of dysprosium. Examples of carbonates of dysprosium include, but are not limited to, dysprosium carbonate. Examples of oxides of dysprosium include, but are not limited to, dysprosium oxide. Examples of oxalates of dysprosium include, but are not limited to, dysprosium oxalate. Examples of hydroxides of dysprosium include, but are not limited to, dysprosium hydroxide. Examples of sulfates of dysprosium include, but are not limited to, dysprosium sulfate.
According to the preparation method of the present invention, preferably, the flux is selected from one or more of boric acid, borate, and alkaline earth metal fluoride. Examples of borates include, but are not limited to, lithium borate. Examples of alkaline earth metal fluorides include, but are not limited to, barium fluoride, magnesium fluoride, calcium fluoride. More preferably, the fluxing agent is selected from boric acid. The dosage of the fluxing agent is 3 to 10 weight percent of the raw material; preferably 4 to 6wt%. Thus, a better fluxing effect can be achieved.
The step (1) may further include a step of tabletting the uniformly mixed substance. This facilitates the shaping of the mixture. In step (2), the reducing atmosphere may be achieved by adding carbon powder. The step (2) further comprises a step of grinding the cooled product.
According to the preparation method of the invention, preferably, in the step (2), the temperature is raised to 1250-1450 ℃ at the temperature raising rate of 2-15 ℃/min, and then the calcination is carried out for 1-5 h. The heating rate can be 2-15 ℃/min; preferably 2 to 8 ℃/min. The calcination temperature can be 1250-1450 ℃; preferably 1300 to 1400 ℃. The calcination time can be 1-5 h; preferably 1 to 3 hours.
The invention unexpectedly discovers that the ammonium bicarbonate can improve the luminous intensity of the yellow-green long afterglow fluorescent material and reduce the afterglow decay rate.
The invention also provides an application of ammonium bicarbonate in improving the luminous intensity of the yellow-green long afterglow fluorescent material or reducing the afterglow decay rate of the yellow-green long afterglow fluorescent material, wherein the yellow-green long afterglow fluorescent material has the composition shown in the formula (1):
Sr1-x-yAl2O4:Eu2+ x,Dy3+ y (1)
wherein x and y each represent Eu2+And Dy3+Molar ratio of (2)<x<1，0<y<1, and x + y<1。
In certain embodiments, the present invention provides the use of ammonium bicarbonate to increase the luminescence intensity of a yellow-green long persistence fluorescent material. In other embodiments, the invention provides the use of ammonium bicarbonate to reduce the decay rate of the afterglow of a greenish yellow long afterglow fluorescent material.
The invention also discloses an application of ammonium bicarbonate in improving the luminous intensity of the yellow-green long-afterglow fluorescent material and reducing the afterglow decay rate of the yellow-green long-afterglow fluorescent material, wherein the yellow-green long-afterglow fluorescent material has the composition shown in the formula (1):
Sr1-x-yAl2O4:Eu2+ x,Dy3+ y (1)
wherein x and y each represent Eu2+And Dy3+Molar ratio of (2)<x<1，0<y<1, and x + y<1。
The use according to the invention preferably comprises the following steps: uniformly mixing the raw material obtained according to the composition of the yellow-green long afterglow fluorescent material, the fluxing agent and the ammonium bicarbonate to obtain a mixture; calcining the mixture in a reducing atmosphere, and cooling a calcined product to obtain a yellow-green long afterglow fluorescent material; wherein the fluxing agent is selected from one or more of boric acid, borate and alkaline earth metal fluoride.
In the present invention, examples of the borate include, but are not limited to, lithium borate. Examples of alkaline earth metal fluorides include, but are not limited to, barium fluoride, magnesium fluoride, calcium fluoride. More preferably, the fluxing agent is selected from boric acid. The dosage of the fluxing agent is 3 to 10 weight percent of the raw material; preferably 4 to 6wt%. Thus, better fluxing effect can be achieved.
According to the use of the present invention, preferably, the amount of ammonium bicarbonate is 3 to 80wt% of the raw material. More preferably, the amount of ammonium bicarbonate is 40 to 60wt% of the starting material. According to one embodiment of the invention, the amount of ammonium bicarbonate is 50wt% of the starting material. Thus being beneficial to improving the luminous intensity of the yellow-green long afterglow fluorescent material and reducing the afterglow decay rate.
In the present invention, 0.001 yarn-over x-over 0.2,0.001 yarn-over y-over 0.1. Preferably, 0.001 yarn-over x yarn-over 0.008,0.001 yarn-over y yarn-over 0.008. Thus being beneficial to improving the luminous intensity of the yellow-green long afterglow fluorescent material.
According to the application of the invention, the temperature is raised to 1250-1450 ℃ at the temperature raising rate of 2-15 ℃/min, and then the calcination is carried out for 1-5 h. The heating rate can be 2-15 ℃/min; preferably 2 to 8 ℃/min. The calcining temperature can be 1250-1450 ℃; preferably 1300 to 1400 ℃. The calcination time can be 1-5 h; preferably 1 to 3 hours.
In the present invention, the raw material of Sr element may be one or more selected from the group consisting of strontium carbonate, strontium oxide, strontium oxalate, strontium hydroxide, and strontium sulfate. Examples of strontium carbonates include, but are not limited to, strontium carbonate. Examples of strontium oxides include, but are not limited to, strontium oxide. Examples of strontium oxalate salts include, but are not limited to, strontium oxalate. Examples of strontium hydroxide include, but are not limited to, strontium hydroxide. Examples of sulfates of strontium include, but are not limited to, strontium sulfate.
In the present invention, the raw material of Al element may be one or more selected from carbonate of aluminum, oxide of aluminum, oxalate of aluminum, hydroxide of aluminum, and sulfate of aluminum. Examples of aluminum carbonates include, but are not limited to, aluminum carbonate. Examples of oxides of aluminum include, but are not limited to, aluminum oxide. Examples of aluminum oxalates include, but are not limited to, aluminum oxalate. Examples of hydroxides of aluminum include, but are not limited to, aluminum hydroxide. Examples of aluminum sulfates include, but are not limited to, aluminum sulfate.
In the present invention, the raw material of Eu element may be selected from one or more of carbonate of europium, oxide of europium, oxalate of europium, hydroxide of europium, and sulfate of europium. Examples of europium carbonates include, but are not limited to, europium carbonate. Examples of oxides of europium include, but are not limited to, europium oxide. Examples of europium oxalate include, but are not limited to, europium oxalate. Examples of europium hydroxides include, but are not limited to, europium hydroxide. Examples of europium sulfates include, but are not limited to, europium sulfate.
In the present invention, the raw material of Dy element may be one or more selected from the group consisting of a carbonate of dysprosium, an oxide of dysprosium, an oxalate of dysprosium, a hydroxide of dysprosium, and a sulfate of dysprosium. Examples of carbonates of dysprosium include, but are not limited to, dysprosium carbonate. Examples of oxides of dysprosium include, but are not limited to, dysprosium oxide. Examples of oxalates of dysprosium include, but are not limited to, dysprosium oxalate. Examples of hydroxides of dysprosium include, but are not limited to, dysprosium hydroxide. Examples of sulfates of dysprosium include, but are not limited to, dysprosium sulfate.
The ammonium bicarbonate is added in the preparation process of the fluorescent material, so that the luminous intensity of the yellow-green long-afterglow fluorescent material is improved, and the afterglow decay rate of the yellow-green long-afterglow fluorescent material is reduced.
Drawings
FIG. 1 is an afterglow attenuation chart of a yellowish green long afterglow fluorescent material obtained in examples 1 to 6 and a comparative example;
FIG. 2 is an afterglow decay pattern of a yellowish green long afterglow fluorescent material obtained in example 6 and a comparative example;
FIG. 3 is the X-ray diffraction pattern of the yellowish green long-afterglow fluorescent material obtained in example 6 and comparative example and the X-ray diffraction peak spectrum of the PDF standard card with card number 74-0794;
FIG. 4 is an excitation spectrum of a yellowish green long afterglow fluorescent material obtained in example 6 and a comparative example;
FIG. 5 is an emission spectrum of a yellowish green long afterglow fluorescent material obtained in example 6 and a comparative example;
FIG. 6 is a scanning electron microscope image obtained by magnifying the yellowish green long-afterglow fluorescent material obtained in the comparative example by 300 times;
FIG. 7 is a scanning electron microscope image of a yellowish green long-afterglow fluorescent material obtained in a comparative example, magnified 1000 times;
FIG. 8 is a scanning electron microscope image obtained by magnifying the yellowish green long-afterglow fluorescent material obtained in example 6 by 300 times;
FIG. 9 is a scanning electron microscope image obtained by magnifying the yellowish green long-afterglow fluorescent material obtained in example 6 by 1000 times;
FIG. 10 is a scanning electron micrograph of the yellowish green long afterglow fluorescent material obtained in example 6, magnified 500 times.
Detailed Description
In the following examples and comparative examples, strontium carbonate was used as a raw material of Sr element, alumina was used as a raw material of Al element, europium oxide was used as a raw material of Eu element, and dysprosium oxide was used as a raw material of Dy element. The reagents used in the examples and comparative examples were all analytical grade (AR) available from Shanghai Aladdin Biotechnology Ltd.
Examples 1 to 6
(1) The fluorescent raw material (shown in table 1) obtained according to the composition of the yellowish green long-afterglow fluorescent material, boric acid and ammonium bicarbonate are uniformly mixed, and then a tablet machine is adopted for tabletting, so that a mixture is obtained.
(2) Heating the mixture to 1350 ℃ in a reducing atmosphere created by carbon powder according to a heating rate of 5 ℃/min, and calcining for 2h to obtain a calcined product; and cooling the calcined product to room temperature, and grinding to obtain the yellow-green long afterglow fluorescent material.
Comparative example
(1) The fluorescent raw material (shown in table 1) obtained according to the composition of the yellow-green long-afterglow fluorescent material and boric acid are uniformly mixed, and then tabletting is carried out by adopting a tabletting machine to obtain a mixture.
(2) Heating the mixture to 1350 ℃ in a reducing atmosphere created by carbon powder according to a heating rate of 5 ℃/min, and calcining for 2h to obtain a calcined product; and cooling the calcined product to room temperature, and grinding to obtain the yellowish green long afterglow fluorescent material.
TABLE 1
Examples of the experiments
The following experimental methods are adopted to test the yellow-green long afterglow fluorescent materials of the examples and the comparative examples, and the specific methods are as follows:
and (3) afterglow testing: and (3) placing the sample to be detected in a dark environment for more than 24h, wherein an excitation light source is a xenon lamp, the irradiation intensity is 1000lx, and the irradiation time is 15min. After 15min excitation is finished, the light source is turned off, the PR-305 type long afterglow phosphor afterglow tester is adopted to detect the luminous intensity of the sample to be detected at different time, and the sampling interval is 1s.
As can be seen from FIG. 1, the addition of ammonium bicarbonate is beneficial to the improvement of the luminescence intensity of the long afterglow fluorescent material. Both the initial luminous intensity and the afterglow intensity after 1 hour are improved to a certain degree. The initial luminous intensity of the long afterglow fluorescent material prepared by adding 50wt% of ammonium bicarbonate reaches the maximum, and after the afterglow decays after 1 hour, the residual glow intensity is more than 2 times of the afterglow intensity of a sample without the ammonium bicarbonate.
As can be seen from FIG. 2, the long afterglow fluorescent material prepared by adding 50wt% ammonium bicarbonate is superior to the sample without ammonium bicarbonate, regardless of the initial luminous intensity or afterglow decay. The long afterglow fluorescent material prepared without adding ammonium bicarbonate has low initial luminous intensity and fast afterglow decay. From the initial luminous intensity to the lowest luminance visible to the human eye (0.32 mcd. M)-2) The time required was about 7h. The long afterglow fluorescent material prepared by adding 50wt% of ammonium bicarbonate is attenuated from the initial luminous intensity to the lowest brightness (0.32 mcd.m) visible to human eyes-2) The time required for (a) was about 9 hours. This indicates that the addition of ammonium bicarbonate increases the luminescence intensity and decreases the decay rate of afterglow.
As can be seen from FIG. 3, the diffraction peak of the long afterglow fluorescent material prepared by adding 50wt% ammonium bicarbonate is substantially consistent with the diffraction peak of the long afterglow fluorescent material prepared without adding ammonium bicarbonate, and the diffraction data is well consistent with the card number 74-0794 PDF standard card. This indicates that the products obtained are all pure SrAl2O4And (4) phase(s). This indicates that the addition of ammonium bicarbonate has no significant effect on the crystal structure of the long persistence phosphor material.
As can be seen from FIGS. 4 and 5, the addition of ammonium bicarbonate has no effect on the excitation spectrum of the long afterglow fluorescent material. Excitation spectrum is continuous wide band spectrum, and belongs to Eu2+The excitation peak is at 370nm. The addition of ammonium bicarbonate improves the luminous intensity of the long afterglow fluorescent material.
As can be seen from FIGS. 6 to 10, the addition of ammonium bicarbonate changes the surface morphology of the long afterglow fluorescent material from flat and dense to convex and porous structures. Thus improving the luminous intensity of the long afterglow fluorescent material and reducing the decay rate of afterglow.
The present invention is not limited to the above-described embodiments, and any variations, modifications, and alterations that may occur to those skilled in the art may fall within the scope of the present invention without departing from the spirit of the present invention.
Claims (10)
1. A preparation method of a yellow-green long afterglow fluorescent material is characterized by comprising the following steps:
(1) Uniformly mixing the raw material obtained according to the composition of the yellow-green long afterglow fluorescent material, boric acid and ammonium bicarbonate to obtain a mixture; the Sr element raw material is strontium carbonate, the Al element raw material is aluminum oxide, the Eu element raw material is europium oxide, and the Dy element raw material is dysprosium oxide;
(2) Calcining the mixture in a reducing atmosphere, and cooling a calcined product to obtain a yellow-green long afterglow fluorescent material;
wherein, the yellow-green long afterglow fluorescent material has the composition shown in formula (1):
Sr1-x-yAl2O4:Eu2+ x,Dy3+ y (1)
wherein x and y each represent Eu2+And Dy3+In a molar ratio of 0<x<1，0<y<1, and x + y<1。
2. The method according to claim 1, wherein the ammonium bicarbonate is used in an amount of 3 to 80wt% based on the raw material.
3. The production method as claimed in claim 1, wherein 0.001 </x </0.2, 0.001 </y </0.1.
4. The method according to claim 1, wherein in the step (2), the temperature is raised to 1250 to 1450 ℃ at a temperature raising rate of 2 to 15 ℃/min, and then the calcination is carried out for 1 to 5 hours.
5. The application of ammonium bicarbonate in improving the luminous intensity or reducing the afterglow decay rate of a yellow-green long afterglow fluorescent material is characterized in that the yellow-green long afterglow fluorescent material has the composition shown in a formula (1):
Sr1-x-yAl2O4:Eu2+ x,Dy3+ y (1)
wherein x and y each represent Eu2+And Dy3+In a molar ratio of 0<x<1，0<y<1, and x + y<1；
The method comprises the following steps: uniformly mixing the raw material obtained according to the composition of the yellow-green long afterglow fluorescent material, boric acid and ammonium bicarbonate to obtain a mixture; calcining the mixture in a reducing atmosphere, and cooling a calcined product to obtain a yellow-green long afterglow fluorescent material; wherein, the raw material of Sr element is strontium carbonate, the raw material of Al element is aluminum oxide, the raw material of Eu element is europium oxide, and the raw material of Dy element is dysprosium oxide.
6. Use according to claim 5, characterized in that the ammonium bicarbonate is used in an amount of 3 to 80% by weight of the starting material.
7. Use according to claim 5, characterized in that the temperature is raised to 1250-1450 ℃ at a ramp rate of 2-15 ℃/min and then calcined for 1-5 h.
8. The application of ammonium bicarbonate in improving the luminous intensity of a yellow-green long afterglow fluorescent material and reducing the afterglow decay rate of the yellow-green long afterglow fluorescent material is characterized in that the yellow-green long afterglow fluorescent material has the composition shown in a formula (1):
Sr1-x-yAl2O4:Eu2+ x,Dy3+ y (1)
wherein x and y each represent Eu2+And Dy3+In a molar ratio of 0<x<1，0<y<1, and x + y<1；
The method comprises the following steps: uniformly mixing the raw material obtained according to the composition of the yellow-green long afterglow fluorescent material, boric acid and ammonium bicarbonate to obtain a mixture; calcining the mixture in a reducing atmosphere, and cooling a calcined product to obtain a yellow-green long afterglow fluorescent material; wherein, the raw material of Sr element is strontium carbonate, the raw material of Al element is aluminum oxide, the raw material of Eu element is europium oxide, and the raw material of Dy element is dysprosium oxide.
9. Use according to claim 8, characterized in that the amount of ammonium bicarbonate is 3-80 wt.% of the starting material.
10. Use according to claim 8, characterized in that the temperature is raised to 1250-1450 ℃ at a ramp rate of 2-15 ℃/min and then calcined for 1-5 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010496461.8A CN111635757B (en) | 2020-06-03 | 2020-06-03 | Preparation method of yellow-green long afterglow fluorescent material and application of ammonium bicarbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010496461.8A CN111635757B (en) | 2020-06-03 | 2020-06-03 | Preparation method of yellow-green long afterglow fluorescent material and application of ammonium bicarbonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111635757A CN111635757A (en) | 2020-09-08 |
| CN111635757B true CN111635757B (en) | 2022-11-01 |
Family
ID=72327670
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010496461.8A Active CN111635757B (en) | 2020-06-03 | 2020-06-03 | Preparation method of yellow-green long afterglow fluorescent material and application of ammonium bicarbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111635757B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113956874B (en) * | 2021-09-24 | 2023-04-18 | 广州珠江光电新材料有限公司 | Long-afterglow fluorescent luminescent material and preparation method thereof |
| CN116285964B (en) * | 2023-03-28 | 2024-04-12 | 阳山金淘精密制品有限公司 | Li (lithium ion battery) + Doped long afterglow luminescent material, li + Preparation method and application of doped long-afterglow luminescent material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1664057A (en) * | 2005-02-21 | 2005-09-07 | 东南大学 | Process for preparing aluminate fluorescent powder by coprecipitation method |
| CN1766033A (en) * | 2005-09-09 | 2006-05-03 | 中国铝业股份有限公司 | Aluminate base long persistence phosphor powder preparation method |
| CN110204321A (en) * | 2019-07-02 | 2019-09-06 | 江苏师范大学 | A kind of light accumulation type diphase ceramic material and preparation method thereof with super brightness |
| CN110467915A (en) * | 2019-04-10 | 2019-11-19 | 济南大学 | A kind of SrAl2O4: Dy3+/Eu2+The synthesis of green long afterglow fluorescent material |
-
2020
- 2020-06-03 CN CN202010496461.8A patent/CN111635757B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1664057A (en) * | 2005-02-21 | 2005-09-07 | 东南大学 | Process for preparing aluminate fluorescent powder by coprecipitation method |
| CN1766033A (en) * | 2005-09-09 | 2006-05-03 | 中国铝业股份有限公司 | Aluminate base long persistence phosphor powder preparation method |
| CN110467915A (en) * | 2019-04-10 | 2019-11-19 | 济南大学 | A kind of SrAl2O4: Dy3+/Eu2+The synthesis of green long afterglow fluorescent material |
| CN110204321A (en) * | 2019-07-02 | 2019-09-06 | 江苏师范大学 | A kind of light accumulation type diphase ceramic material and preparation method thereof with super brightness |
Non-Patent Citations (1)
| Title |
|---|
| Synthesis of M1-3xAl2O4:Eu2+x/Dy3+2x (M2+=Sr2+,Ca2+ and Ba2+) phosphors with long-lasting phosphorescence properties via co-precipitation method;Jinkai Li et al.;《Chem Rep》;20190711;第1卷(第2期);第112-117页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111635757A (en) | 2020-09-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR100304167B1 (en) | Long afterglow light emitting material and its manufacturing method | |
| CN111635757B (en) | Preparation method of yellow-green long afterglow fluorescent material and application of ammonium bicarbonate | |
| CN107974250B (en) | Blue-green silicate ultra-long afterglow luminescent material and preparation method thereof | |
| CN113817465A (en) | Bismuth ion doped germanate base orange long afterglow material and preparation method thereof | |
| JP6292684B1 (en) | Luminescent phosphor and method for producing the same | |
| CN109370580B (en) | Bismuth ion activated titanium aluminate fluorescent powder and preparation method and application thereof | |
| CN102666783B (en) | Borate luminous material and preparation method thereof | |
| JP2006152242A (en) | Luminous material and process for producing the same | |
| WO2011033830A1 (en) | Phosphor | |
| JPH1161114A (en) | Light-emitting material for high-speed excitation, high brilliance, and low attenuation, and its production | |
| CN107722972B (en) | Green long-afterglow luminescent material and preparation method thereof | |
| JPH09143464A (en) | High-luminance long-afterglow phosphorescent material and its production | |
| RU2506301C2 (en) | Luminescent material for solid-state white light sources | |
| CN106147767B (en) | A kind of long after glow luminous material and preparation method thereof | |
| CN103361053A (en) | Silicate luminous material and preparation method thereof | |
| CN109233826B (en) | Europium ion activated titanium aluminate fluorescent powder and preparation method and application thereof | |
| EP2565253B1 (en) | Silicate luminescent material and production method thereof | |
| CN105860971A (en) | Rare earth ion doped zirconium niobate fluorescent powder and preparation method thereof | |
| CN102533269B (en) | Fluorescent material for solid white light source and preparation method thereof | |
| CN106978177B (en) | Red long afterglow luminescent material and production method thereof | |
| CN101372617A (en) | Blue fluorescent powder for field emission and vacuum fluorescence display and preparation thereof | |
| CN116120923B (en) | Eu in Eu 2+ Activated alkali metal haloborate fluorescent powder and preparation method and application thereof | |
| CN103627393A (en) | Tungsten molybdate red phosphor powder and preparation method and application thereof | |
| JP6741614B2 (en) | Rare earth activated alkaline earth silicate compound Afterglow phosphor | |
| JP2004359701A (en) | Light-accumulating phosphor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |