CN110467915A - A kind of SrAl2O4: Dy3+/Eu2+The synthesis of green long afterglow fluorescent material - Google Patents
A kind of SrAl2O4: Dy3+/Eu2+The synthesis of green long afterglow fluorescent material Download PDFInfo
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- CN110467915A CN110467915A CN201910283261.1A CN201910283261A CN110467915A CN 110467915 A CN110467915 A CN 110467915A CN 201910283261 A CN201910283261 A CN 201910283261A CN 110467915 A CN110467915 A CN 110467915A
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- fluorescent material
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- 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
Abstract
The invention discloses a kind of SrAl2O4: Dy3+/Eu2+The synthetic method of green long afterglow fluorescent material, chemical formula group become Sr0.55Al2O4: Dy3+ 0.3/Eu2+ 0.15, which is to be mixed in a certain ratio to obtain female salt with strontium nitrate, dysprosium nitrate, gadolinium nitrate, europium nitrate and aluminum nitrate, and it is added drop-wise to dropwise in the certain density ammonium bicarbonate soln of configuration.After being added dropwise, when validity response 30 minutes, obtain precursor powder after being centrifuged, washed and being dried, eventually pass through under reducing atmosphere calcining obtain SrAl2O4: Dy3+/Eu2+Green long afterglow fluorescent material.Long lad phosphor fluorescence property prepared by the present invention is excellent, be expected to fluorescent powder of new generation apply illumination and cell display field in play an important role.
Description
Technical field
The present invention relates to a kind of preparations of green long afterglow fluorescent material applied to the fields such as illumination and display, have
Single fluorescence emission peak, and there is apparent twilight sunset phenomenon.
Background technique
Since long after glow luminous material can release in the form of light the energy of absorption, in Emergency Light, instrument
Table shows, security against fire, building decoration, high-energy ray detection, the lossless detection of engineering ceramics, fibre optic thermometer and military installations
Equal fields are widely used.It can be applied to new energy, life with the development of science and technology, being expected to obtain in the near future
The sciemtifec and technical spheres such as science, information processing.With the development of new and high technology, people to the luminous efficiency of fluorescent powder, stability and
Particle size has also been proposed higher requirement.Although aluminate series long afterglow fluorescent material has good luminous performance, chemical property steady
The advantages that determining, can be used for a long time in air, being a kind of energy-saving and environment-friendly advanced luminescent material developed rapidly in recent years,
But still it is not able to satisfy the application in the fields such as optical instrument and Emergency Light, the long-afterglow fluorescent material for developing higher performance seems
It is extremely urgent.
The fluorescence property of fluorescent material and particle size, pattern and crystallinity etc. are closely related.Due to utilizing solid phase legal system
The disadvantages of that there are particle shapes is different for standby fluorescent powder, size is uneven and crystallinity is not good enough, seriously affect its in illumination and
The application in the fields such as display.So preparing size uniformity and the length with excellent fluorescence property using ammonium hydrogen carbonate coprecipitation
Twilight sunset fluorescent material has great importance.
Summary of the invention
Problem to be solved of the present invention is, using ammonium hydrogen carbonate coprecipitation, by the doping for adjusting Eu2+ and Dy3+
Concentration is prepared for the green long afterglow fluorescent material with single emission peak.
In order to achieve the above object, the present invention uses following scheme:
A kind of SrAl2O4: Dy3+/Eu2+The synthesis of green long afterglow fluorescent material, preparation method the following steps are included:
(1) by rare earth oxide (Dy2O3And Eu2O3) be dissolved in hot nitric acid and be configured to rare earth nitrades；
(2) by Sr2+、Al3+、Dy3+And Eu3+In molar ratio for 1-3x:2:2x:x (x=0.15) measure rare earth nitrades, with go from
Sub- water supplement makes solution reach 100mL, is uniformly mixed and obtains female salt；
(3) ammonium hydrogen carbonate of 23.88 g is weighed, so that solution is reached 200mL with deionized water supplement, configures certain density carbonic acid
Hydrogen ammonium salt solution；
(4) female salt of step 2 is added drop-wise to dropwise in the ammonium bicarbonate soln of step 3, after being added dropwise, reacts at room temperature 30min；
(5) suspension after step 4 reaction is centrifuged, is washed and is dried to obtain white precursor powder；
(6) by the presoma in step 5 through calcining to obtain SrAl under reducing atmosphere2O4: Dy3+/Eu2+Long-afterglow fluorescent material.
Detailed description of the invention
Fig. 1 is through 1300。The Sr obtained after C1-3xAl2O4: Dy3+ 2x/Eu2+ x(x=0.05-0.3) fluorescent powder swashs in 360nm
The emission spectrum given；Embedded figure be under 519nm fluorescence intensity with Eu2+The variation of doping and change.
Fig. 2 is through 1300。The Sr obtained after C0.55Al2O4: Dy3+ 0.3/Eu2+ 0.15Twilight sunset of the fluorescent powder under 360nm excitation
Life diagram.
Below by specific example, the present invention is further explained.
Example one
A kind of SrAl2O4: Dy3+/Eu2+The synthesis of green long afterglow fluorescent material, preparation method the following steps are included:
(1) by rare earth oxide (Dy2O3And Eu2O3) be dissolved in hot nitric acid and be configured to rare earth nitrades；
(2) by Sr2+、Al3+、Dy3+And Eu3+Rare earth nitrades are measured for 0.75:2:0.1:0.05 in molar ratio, with deionized water
Supplement makes solution reach 100mL, is uniformly mixed and obtains female salt；
(3) ammonium hydrogen carbonate of 23.88 g is weighed, so that solution is reached 200mL with deionized water supplement, configures certain density carbonic acid
Hydrogen ammonium salt solution；
(4) female salt of step 2 is added drop-wise to dropwise in the ammonium bicarbonate soln of step 3, after being added dropwise, reacts at room temperature 30min；
(5) suspension after step 4 reaction is centrifuged, is washed and is dried to obtain white precursor powder；
(6) by the presoma in step 5 through calcining to obtain SrAl under reducing atmosphere2O4: Dy3+/Eu2+Long-afterglow fluorescent material.
Example two
The implementation steps of the implementation case and example one the difference is that, by the Sr in step (2)2+、Al3+、Dy3+And Eu3 +Molar ratio is changed to 0.7:2:0.2:0.1, and other conditions are identical as example one.
Example three
The implementation steps of the implementation case and example one the difference is that, by the Sr in step (2)2+、Al3+、Dy3+And Eu3 +Molar ratio is changed to 0.65:2:0.3:0.15, and other conditions are identical as example one.
Example four
The implementation steps of the implementation case and example one the difference is that, by the Sr in step (2)2+、Al3+、Dy3+And Eu3 +Molar ratio is changed to 0.4:2:0.4:0.2, and other conditions are identical as example one.
Example five
The implementation steps of the implementation case and example one the difference is that, by the Sr in step (2)2+、Al3+、Dy3+And Eu3 +Molar ratio is changed to 0.25:2:0.5:0.25, and other conditions are identical as example one.
Example six
The implementation steps of the implementation case and example one the difference is that, by the Sr in step (2)2+、Al3+、Dy3+And Eu3 +Molar ratio is changed to 0.1:2:0.6:0.3, and other conditions are identical as example one.
Fig. 1 reflection is different Eu2+And Dy3+Doping to SrAl2O4: Dy3+/Eu2+The fluorescence of long-afterglow fluorescent material
The influence of performance.On the one hand, You Tuzhong is it is found that in Eu2+360nm excitation wavelength under, it can be seen that at 519nm exist
Eu2+Single green emission (4f65d1→4f7Transition), and by embedded figure it can be seen that with Eu2+Volume increase,
Fluorescence intensity presentation first increases the trend reduced afterwards, i.e. Eu2+The optimum mix amount be 15% at..On the other hand, with Dy3+And Eu2 +, there is not Dy in the increase of volume3+Emission peak, this explanation in the system Dy3+Play a part of to be sensitized and stablize lattice.
Fig. 2 reaction is the SrAl for utilizing Co deposited synthesis2O4: Dy3+/Eu2+The twilight sunset service life of long-afterglow fluorescent material,
As seen from the figure, the twilight sunset service life can achieve 31.59 min.
Claims (6)
1. a kind of SrAl2O4: Dy3+/Eu2+The synthesis of green long afterglow fluorescent material, it is characterised in that its chemical formula forms Sr1- 3xAl2O4: Dy3+ 2x/Eu2+ x, wherein x=0.05-0.3.
2. a kind of SrAl according to claim 12O4: Dy3+/Eu2+The synthesis of green long afterglow fluorescent material, feature
It is, comprising the following steps:
(1) by rare earth oxide (Dy2O3And Eu2O3) be dissolved in hot nitric acid and be configured to rare earth nitrades；
(2) by Sr2+、Al3+、Dy3+And Eu3+In molar ratio for 1-3x:2:2x:x (x=0.15) measure rare earth nitrades, with go from
Sub- water supplement makes solution reach 100mL, is uniformly mixed and obtains female salt；
(3) a certain amount of ammonium hydrogen carbonate is weighed, so that solution is reached 200mL with deionized water supplement, configures certain density carbonic acid
Hydrogen ammonium salt solution；
(4) female salt of step 2 is added drop-wise to dropwise in the ammonium bicarbonate soln of step 3, after being added dropwise, reacts at room temperature 30min；
(5) suspension after step 4 reaction is centrifuged, is washed and is dried to obtain white precursor powder；
(6) by the presoma in step 5 through calcining to obtain SrAl under reducing atmosphere2O4: Dy3+/Eu2+Green long afterglow phosphor
Material.
3. preparation method as claimed in claim 2, which is characterized in that Eu2+Optium concentration be 0.15M.
4. preparation method as claimed in claim 2, which is characterized in that Dy3+Optium concentration be 0.3M.
5. preparation method as claimed in claim 2, which is characterized in that the concentration of ammonium bicarbonate soln is 1.5M.
6. preparation method as claimed in claim 2, which is characterized in that the calcining of presoma is to calcine (M under reducing atmosphereH2:
MN2=1:4) to 1300。C keeps the temperature 4h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111518550A (en) * | 2020-03-05 | 2020-08-11 | 济南大学 | Functional filler with gelling and long-afterglow luminescent characteristics and preparation method and application thereof |
| CN111635757A (en) * | 2020-06-03 | 2020-09-08 | 重庆交通大学 | Preparation method of yellow-green long-afterglow fluorescent material and application of ammonium bicarbonate |
| CN113831916A (en) * | 2021-10-11 | 2021-12-24 | 中国人民解放军陆军工程大学 | Preparation method of rare earth doped long-afterglow luminescent material |
| RU2797662C1 (en) * | 2022-06-27 | 2023-06-07 | Акционерное общество "Научно-производственное предприятие "Интеграл" | Photostimulated luminescent compound |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111518550A (en) * | 2020-03-05 | 2020-08-11 | 济南大学 | Functional filler with gelling and long-afterglow luminescent characteristics and preparation method and application thereof |
| CN111635757A (en) * | 2020-06-03 | 2020-09-08 | 重庆交通大学 | Preparation method of yellow-green long-afterglow fluorescent material and application of ammonium bicarbonate |
| CN111635757B (en) * | 2020-06-03 | 2022-11-01 | 重庆交通大学 | Preparation method of yellow-green long afterglow fluorescent material and application of ammonium bicarbonate |
| CN113831916A (en) * | 2021-10-11 | 2021-12-24 | 中国人民解放军陆军工程大学 | Preparation method of rare earth doped long-afterglow luminescent material |
| RU2797662C1 (en) * | 2022-06-27 | 2023-06-07 | Акционерное общество "Научно-производственное предприятие "Интеграл" | Photostimulated luminescent compound |
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Application publication date: 20191119 |