CN106978173A - A kind of orthosilicate base red fluorescent powder and preparation method thereof - Google Patents
A kind of orthosilicate base red fluorescent powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of orthosilicate base red fluorescent powder and preparation method thereof, belong to a kind of phosphor and display technology field, to achieve the above objectives, the technical solution adopted by the present invention is to provide a kind of Eu3+The orthosilicate base red fluorescent powder of activation, its chemical formula is Li2Mg1‑xEuxSiO4, wherein, x is Eu3+The mole percent of doping, 0.0001≤x≤0.05.Described fluorescent material launches feux rouges of the wavelength at 570~725 nanometers in the case where wavelength excites for 250~490 nanometers ultraviolet to blue light.The preparation method of the present invention uses high temperature solid-state method or sol-gal process, and orthosilicate base red fluorescent powder prepared by the present invention has good heat endurance, colour rendering and granularity, is advantageously implemented and prepares high-power LED.
Description
Technical field
The invention belongs to a kind of phosphor and display technology field, a kind of Eu is specifically related to3+The positive silicon of activation
Sour magnesium lithium red fluorescence powder and preparation method thereof.
Background technology
LED (Light Emitting Diode) is used as the green illumination light source of a new generation, extensive use
In lighting field, especially white light LEDs, with power consumption is few, service life length, operating voltage is low, performance is stable, impact resistance
By force, the advantage such as small volume, cost low, luminescence response is fast, energy-conserving and environment-protective, thus more and more extensive attention has been obtained with studying,
Particularly blueness, purple and near ultraviolet LED are developed rapidly in recent years, the LED is replaced incandescent lamp and fluorescent lamp in lighting field
It is possibly realized.
Rare-earth trichromatic fluorescent powder is the main raw material(s) for producing energy-efficient lamp, compared with ordinary incandescent lamp, section
Electric rate is up to 80%, and can obtain the colour temperature close with daylight so that illuminated object pure color is undistorted, and it was produced
Journey is environmentally safe, is putative ideal green illuminating engineering.Rare-earth trichromatic fluorescent lamp is glimmering using red, blue, green three kinds
Light powder.At present, yellow both domestic and external and green emitting phosphor are very ripe in package application, and red fluorescence powder is existed surely
The low defect of qualitative poor, efficiency, the bottleneck lighted as white light LEDs.
At present, it is commercialized that sulfide and nitride are still confined to based on the red fluorescence powder that blue-light LED chip is excited
System.Sulfide systems are less efficient, poor chemical stability, are also easy to produce H2S gases and corrode LED chip;Though Nitride systems
So overcome the disadvantages mentioned above of sulfide and show preferable performance, but its higher price makes most of LED encapsulation factories
Business can not bear and limit its application.Therefore a kind of stability is developed high, price is low, can be had by black light/blue light
The red fluorescence powder excited is imitated by industry deepest concern.
Silicate systems luminescent material has good chemical stability and heat endurance, and low raw-material cost, prepares
Technique is simple.It overcomes sulfide or the labile deficiency of oxysulfide red fluorescence powder, and synthesis temperature is far below nitridation
Thing red fluorescence powder, is increasingly becoming the focus of research.Eu3+Doped silicate red fluorescence powder report is more, and such as Chinese invention is special
Profit 201310087864.7 provides a kind of europium ion Eu3+The silicate-base luminescent material of activation, preparation method and application, it is changed
Formula is:Na9Y1-xEuxSi6O18, wherein 0.0001≤x≤0.5.But Eu3+Adulterate Li2MgSiO4So far there are no for red fluorescence powder
Report.
The content of the invention
It is an object of the invention to provide a kind of orthosilicate base red fluorescent powder and preparation method thereof, the orthosilicate base
Red fluorescence powder chemistry and stable optical performance, preparation technology are easy, mild condition, environmental protection, and can reduce energy consumption and into
This Eu3+The silicate-base luminescent material of activation, preparation method and applications, are that this area increases the new kind of a class, are promoted
The extensive use of phosphor.
To achieve the above objectives, the technical solution adopted by the present invention is to provide a kind of Eu3+The orthosilicate base of activation is red
Fluorescent material, its chemical formula is Li2Mg1-xEuxSiO4, wherein, x is Eu3+The mole percent of doping, 0.0001≤x≤0.05.
Described fluorescent material launches wavelength at 570~725 nanometers in the case where wavelength excites for 250~490 nanometers ultraviolet to blue light
Feux rouges.
Technical solution of the present invention provides a kind of Eu as described above3+The method of the orthosilicate base red fluorescent powder of activation,
Using high temperature solid-state method, comprise the following steps:
(1) to contain magnesium ion Mg2+Compound, contain lithium ion Li+Compound, contain europium ion Eu3+Chemical combination
Thing and silica are raw material, by molecular formula Li2Mg1-xEuxSiO4The stoichiometric proportion of middle corresponding element weighs each raw material, will claim
The raw mill taken is well mixed, and obtains mixture;
(2) said mixture is calcined for the first time in air atmosphere, calcining heat is 300~450 DEG C, and calcination time is
5~8 hours;
(3) by the mixture natural cooling after calcining, grind and be well mixed, second of sintering in air atmosphere burns
Junction temperature is 750~1300 DEG C, and sintering time is 8~15 hours.After natural cooling, a kind of Eu is obtained3+The orthosilicate of activation
Base red fluorescent powder.
In high temperature solid-state method, the calcining heat described in step (2) is preferably 350~400 DEG C, and calcination time is preferably 5
~6 hours;Calcining heat described in step (3) is preferably 850~950 DEG C, and calcination time is preferably 10~12 hours.
Technical solution of the present invention also includes providing a kind of europium ion Eu as described above3+The orthosilicate base fluorescent powder of activation
Preparation method, using sol-gel process, comprise the following steps:
(1) with Eu containing europium ion3+Compound, Li containing lithium ion+Compound, Mg containing magnesium ion2+Compound for original
Material, by formula Li2Mg1-xEuxSiO4The stoichiometric proportion of middle corresponding element weighs each raw material, and wherein x is Eu3+Moles the hundred of doping
Fraction, 0.0001≤x≤0.05.Each raw material is dissolved separately in dilute nitric acid solution, diluted with deionized water, then by each raw material
0.5~2.0wt% of middle reactant quality adds complexing agent respectively, obtains the solution of each raw material, and obtained each solution is mixed
Uniformly;Described complexing agent is one kind in citric acid, oxalic acid;
(2) formula Li is pressed2Mg1-xEuxSiO4The chemistry mole metering ratio of middle corresponding element weighs tetraethyl orthosilicate, by positive silicon
Acetoacetic ester is added in absolute ethyl alcohol, well mixed to obtain teos solution;
(3) mixed solution for obtaining step (1) is added to the teos solution that step (2) is prepared, mixing
Uniformly.Above-mentioned mixed solution is stirred 5~10 hours under 60~80 DEG C of water bath condition, vitreosol is obtained after standing;
(4) vitreosol obtained by obtains precursor powder after 100 DEG C of drying form xerogel, grinding;
(5) by the pre-burning in air atmosphere of obtained precursor powder, calcined temperature is 300~450 DEG C, and sintering time is
5~20 hours;
(6) after natural cooling, grind and be well mixed, sintered in air atmosphere, sintering temperature is 700~1000 DEG C,
Sintering time is 5~20 hours.A kind of europium ion Eu is obtained after natural cooling3+The orthosilicate base red fluorescent powder of activation.
In chemical solution method, the calcined temperature described in step (5) is preferably 350~400 DEG C, and sintering time is preferably 10
~15 hours;Sintering temperature described in step (6) is preferably 750~850 DEG C, and sintering time is preferably 10~15 hours.
Contain magnesium ion Mg described in technical solution of the present invention2+Compound include magnesia, magnesium hydroxide, magnesium carbonate,
One kind in basic magnesium carbonate, magnesium nitrate.Described contains lithium ion Li+Compound include lithium carbonate, lithium hydroxide, nitric acid
One kind in lithium.Described contains europium ion Eu3+Compound be europium oxide, europium nitrate in one kind.
Beneficial effect:
(1) the invention provides a kind of new orthosilicate base red fluorescent powder, it can be at 250~490 nanometers
It is ultraviolet to be excited down to blue light, feux rouges of the main peak at 613 nanometers is sent, red degree is pure, near ultraviolet LED chip and blue-ray LED
Chip output wavelength matching is good, can be applicable to white light LEDs field.
(2) orthosilicate base red fluorescent powder raw material sources prepared by the present invention enrich, cheap, preparation technology letter
It is single, it is easy to operate, and the requirement to equipment is low, the production cost of product is low;Compared with other sulfide, halide, in production
Without waste water and gas discharge, environmental protection.
(3) orthosilicate base red fluorescent powder prepared by the present invention has good heat endurance, colour rendering and granularity, has
High-power LED is prepared beneficial to realizing.
Brief description of the drawings
Fig. 1 is the X-ray powder diffraction pattern of the material sample prepared by the technical scheme of the embodiment of the present invention 1;
Fig. 2 is the scanning electron microscope (SEM) photograph of the material sample prepared by the technical scheme of the embodiment of the present invention 1;
Fig. 3 is luminous light of the material sample prepared by the technical scheme of the embodiment of the present invention 1 in the case where 393 nanometers of light is excited
Spectrogram;
Fig. 4 be by the technical scheme of the embodiment of the present invention 1 prepare material sample obtained under 613 nanometers of light detection it is near
The exciting light spectrogram of ultraviolet region;
Fig. 5 is that the material sample prepared by the technical scheme of the embodiment of the present invention 1 is 393 nanometers in excitation wavelength, monitors ripple
A length of 613 nanometers of decay of luminescence curve.
Embodiment
Technical solution of the present invention is further described with reference to the accompanying drawings and examples.
Embodiment 1:
Prepare Li2Mg0.07Eu0.03SiO4
According to chemical formula Li2Mg0.07Eu0.03SiO4The stoichiometric proportion of middle each element, weighs Li respectively2CO3:1.5825
Gram, 4MgCO3·Mg(OH)2·5H2O:2.0178 gram, SiO2:1.2867 gram, Eu2O3:0.1131 gram.Ground in agate mortar
And after being well mixed, calcined for the first time in air atmosphere, temperature is 400 DEG C, and then calcination time 5 hours naturally cools to room
Temperature, takes out sample.Mixing abrasive lapping after first time is calcined simultaneously is well mixed, and second calcines in air atmosphere, calcining
Temperature is 900 DEG C, and calcination time is 10 hours, then naturally cools to room temperature, that is, obtains target product.
Referring to accompanying drawing 1, it is the X-ray powder diffraction pattern of the material sample prepared by the present embodiment technical scheme.XRD
Test result shows that prepared material principal phase is Li2MgSiO4Material.
Referring to accompanying drawing 2, it is the material sample scanning electron microscope (SEM) photograph prepared by the present embodiment technical scheme.SEM test results
It has been shown that, prepared material granule particle diameter is in 0.57 microns, complete crystallization.
Referring to accompanying drawing 3, it is the material sample prepared by the present embodiment technical scheme in 393 nanometers of hairs obtained under exciting
Light spectrum.It can be seen that main peak is located at 613 nms.Calculated by CIE, the chromaticity coordinates for learning it is x=
0.653, y=0.345, just fall in red area, it can be applied to the white light LEDs that black light is excitation source very well.
Referring to accompanying drawing 4, it is by swashing that the material sample of the present embodiment technical scheme preparation is obtained under 613 nanometers of monitorings
Luminous spectrogram.It can be seen that the blue colour fluorescent powder has strong absorption in 250-490 nanometer ranges, can be fine
Ground matches the White-light LED chip of near ultraviolet excitation.
Referring to accompanying drawing 5, it is the decay of luminescence curve of the sample prepared by the present embodiment technical scheme, and the curve presents double
Exponential damping, luminescent lifetime is respectively 0.005 microsecond and 1.515 milliseconds.
Embodiment 2:
Prepare Li2Mg0.999Eu0.001SiO4
According to chemical formula Li2Mg0.999Eu0.001SiO4The stoichiometric proportion of middle each element, weighs LiOH respectively:0.5178
Gram, Mg (OH)2:1.2603 gram, SiO2:1.2994 grams, Eu (NO3)3:0.0073 gram.Grind and be well mixed in agate mortar
Afterwards, calcined for the first time in air atmosphere, temperature is 300 DEG C, calcination time 8 hours, then naturally cool to room temperature, take out sample
Product.Mixing abrasive lapping after first time is calcined simultaneously is well mixed, and second calcines in air atmosphere, and calcining heat is 900
DEG C, calcination time is 12 hours, then naturally cools to room temperature, that is, obtains target product.Its main structure, excitation spectrum,
Luminescent spectrum and decay of luminescence are similar to Example 1.
Embodiment 3:
Prepare Li2Mg0.99Eu0.01SiO4
According to chemical formula Li2Mg0.99Eu0.01SiO4The stoichiometric proportion of middle each element, weighs LiNO respectively3:2.9734 gram,
Mg(NO3)2:3.1593 gram, SiO2:1.2955 gram, Eu2O3:0.0379 gram.After grinding and be well mixed in agate mortar,
Air atmosphere is calcined for the first time, and temperature is 350 DEG C, calcination time 7 hours, then naturally cools to room temperature, takes out sample.
Mixing abrasive lapping after once calcining simultaneously is well mixed, and second calcines in air atmosphere, and calcining heat is 1000 DEG C, calcining
Time is 15 hours, then naturally cools to room temperature, that is, obtains target product.Its main structure, excitation spectrum, luminescent spectrum
It is similar to Example 1 with decay of luminescence.
Embodiment 4:
Prepare Li2Mg0.95Eu0.05SiO4
According to chemical formula Li2Mg0.95Eu0.05SiO4The stoichiometric proportion of middle each element, weighs Li respectively2CO3:1.5719
Gram, 4MgCO3·Mg(OH)2·5H2O:1.9629 gram, Eu2O3:0.1872 gram.First by the Li weighed2CO3With appropriate deionization
Water, nitric acid dissolving stirring are complete to dissolving, and add appropriate citric acid, and stir process is complete to dissolving;It will weigh again
4MgCO3·Mg(OH)2·5H2O and Eu2O3Handle, i.e., first stirred with appropriate deionized water, nitric acid dissolving, extremely in the same way
Dissolving is added completely into appropriate citric acid, and stir process dissolving is complete;Finally above-mentioned three kinds of solution is mixed, then adds one wherein
Quantitative citric acid stirring obtains mixed solution.Meanwhile, weigh tetraethyl orthosilicate:4.4319 grams, appropriate absolute ethyl alcohol is added, is stirred
Mix to being completely dissolved, obtain teos solution.Above-mentioned mixed solution is mixed with teos solution, stirred.
With being stirred 4 hours under 70 DEG C of water bath condition, vitreosol is obtained after standing.After vitreosol is dried, obtain it is fluffy before
Drive body.First time calcined temperature is 350 DEG C, and sintering time is 15 hours;Second of sintering temperature is 850 DEG C, and sintering time is
15 hours, powder shaped orthosilicate base red fluorescent powder material is obtained after natural cooling.Its main structure, excitation spectrum,
Luminescent spectrum and decay of luminescence are similar to Example 1.
Embodiment 5:
Prepare Li2Mg0.995Eu0.005SiO4
According to chemical formula Li2Mg0.995Eu0.005SiO4The stoichiometric proportion of middle each element, weighs LiNO respectively3:2.9784
Gram, Mg (NO3)2:3.1806 grams, Eu (NO3)3:0.0365 gram.First by the LiNO weighed3Stirred with appropriate deionized water dissolving
It is complete to dissolving, appropriate citric acid is added, stir process is complete to dissolving;Again by the Mg (NO weighed3)2With Eu (NO3)3With phase
With method processing, i.e., stirred with appropriate deionized water dissolving, be added completely into appropriate citric acid to dissolving, stir process has dissolved
Entirely;Finally above-mentioned three kinds of solution is mixed, then adds a certain amount of citric acid stirring wherein and obtains mixed solution.Meanwhile, claim
Take tetraethyl orthosilicate:4.4998 grams, appropriate absolute ethyl alcohol is added, stirs to being completely dissolved, obtains teos solution.Will be upper
State mixed solution to mix with teos solution, stir.With being stirred 3 hours under 75 DEG C of water bath condition, after standing
To vitreosol.After vitreosol is dried, fluffy presoma is obtained.First time calcined temperature is 400 DEG C, and sintering time is
10 hours;Second of sintering temperature is 800 DEG C, and sintering time is 8 hours, and powder shaped orthosilicate base is obtained after natural cooling
Red fluorescence powder material.Its main structure, excitation spectrum, luminescent spectrum and decay of luminescence are similar to Example 1.
Embodiment 6:
Prepare Li2Mg0.9999Eu0.0001SiO4
According to chemical formula Li2Mg0.9999Eu0.0001SiO4The stoichiometric proportion of middle each element, weighs LiOH respectively:1.0358
Gram, 4MgCO3·Mg(OH)2·5H2O:2.1012 grams, Eu (NO3)3:0.0008 gram.First by the LiOH weighed with it is appropriate go from
Sub- water, nitric acid dissolving stirring are complete to dissolving, and add appropriate citric acid, and stir process is complete to dissolving;It will weigh again
4MgCO3·Mg(OH)2·5H2O is handled in the same way, i.e., first stirred with appropriate deionized water, nitric acid dissolving, to having dissolved
Appropriate citric acid is added entirely, and stir process dissolving is complete;Then by the Eu (NO weighed3)3Stirred with appropriate deionized water dissolving
It is complete to dissolving, appropriate citric acid is added, stir process is complete to dissolving;Finally above-mentioned three kinds of solution is mixed, then wherein
Add a certain amount of citric acid stirring and obtain mixed solution.Meanwhile, weigh tetraethyl orthosilicate:4.5071 grams, add appropriate anhydrous
Ethanol, stirs to being completely dissolved, obtains teos solution.Above-mentioned mixed solution is mixed with teos solution, stirred
Mix uniform.With being stirred 3 hours under 80 DEG C of water bath condition, vitreosol is obtained after standing.After vitreosol is dried, obtain fluffy
The presoma of pine.First time calcined temperature is 450 DEG C, and sintering time is 12 hours;Second of sintering temperature is 750 DEG C, sintering
Time is 12 hours, and powder shaped orthosilicate base red fluorescent powder material is obtained after natural cooling.Its main structure, excite
Spectrum, luminescent spectrum and decay of luminescence are similar to Example 1.
Claims (7)
1. a kind of orthosilicate base red fluorescent powder, it is characterised in that:The chemical formula of described orthosilicate base red fluorescent powder
For Li2Mg1-xEuxSiO4, wherein, x is Eu3+The mole percent of doping, 0.0001≤x≤0.05;Described fluorescent material is in ripple
A length of 250~490 nanometers ultraviolet is excited down to blue light, launches feux rouges of the wavelength at 570~725 nanometers.
2. orthosilicate base red fluorescent powder according to claim 1, it is characterised in that:Described orthosilicate base is red
The chemical formula of fluorescent material is:Li2Mg0.97Eu0.03SiO4。
3. the preparation method of orthosilicate base red fluorescent powder according to claim 1, it is characterised in that including following step
Suddenly:
(1) to contain magnesium ion Mg2+Compound, contain lithium ion Li+Compound, contain europium ion Eu3+Compound and
Silica is raw material, by molecular formula Li2Mg1-xEuxSiO4The nonstoichiometric molar ratio of middle corresponding element weighs each raw material, wherein
X is Eu3+The mole percent of doping, the raw mill weighed is well mixed, obtains mixture by 0.0001≤x≤0.05;
(2) said mixture is calcined for the first time in air atmosphere, calcining heat is 300~450 DEG C, calcination time is 5~8
Hour;
(3) by the mixture natural cooling after calcining, grind and be well mixed, second of sintering in air atmosphere, sintering temperature
Spend for 750~1300 DEG C, sintering time is 8~15 hours, after natural cooling, that is, obtains a kind of Eu3+The orthosilicate base of activation
Red fluorescence powder.
4. preparation method according to claim 3, it is characterised in that:In described step (2), described calcining heat is
350~400 DEG C, calcination time is 5~6 hours;In described step (3), described calcining heat is 850~950 DEG C, calcining
Time is 10~12 hours.
5. a kind of preparation method of orthosilicate base fluorescent powder as claimed in claim 1, it is characterised in that:Using colloidal sol-solidifying
Glue method, comprises the following steps:
(1) with Eu containing europium ion3+Compound, Li containing lithium ion+Compound, Mg containing magnesium ion2+Compound be raw material, press
Formula Li2Mg1-xEuxSiO4The chemistry mole metering of middle corresponding element is Eu than weighing each raw material, wherein x3+Moles the hundred of doping
Each raw material is dissolved separately in dilute nitric acid solution, diluted with deionized water by fraction, 0.0001≤x≤0.05, then by each raw material
0.5~2.0wt% of middle reactant quality adds complexing agent respectively, obtains the solution of each raw material, and obtained each solution is mixed
Uniformly;Described complexing agent is one kind in citric acid, oxalic acid;
(2) formula Li is pressed2Mg1-xEuxSiO4The chemistry mole metering ratio of middle corresponding element weighs tetraethyl orthosilicate, by positive silicic acid second
Ester is added in absolute ethyl alcohol, well mixed to obtain teos solution;
(3) mixed solution for obtaining step (1) is added to the teos solution that step (2) is prepared, and is well mixed,
Above-mentioned mixed solution is stirred 5~10 hours under 60~80 DEG C of water bath condition, vitreosol is obtained after standing;
(4) vitreosol obtained by is dried to form xerogel, and precursor powder is obtained after grinding;
(5) by the pre-burning in air atmosphere of obtained precursor powder, calcined temperature be 300~450 DEG C, sintering time be 5~
20 hours;
(6) after natural cooling, grind and be well mixed, sintered in air atmosphere, sintering temperature is 700~1000 DEG C, sintering
Time is 5~20 hours, and a kind of europium ion Eu is obtained after natural cooling3+The orthosilicate base red fluorescent powder of activation.
6. the preparation method of orthosilicate base fluorescent powder according to claim 5, it is characterised in that:Described step (5)
In, described calcined temperature is 350~400 DEG C, and sintering time is 10~15 hours;In described step (6), described sintering
Temperature is 750~850 DEG C, and sintering time is 10~15 hours.
7. the preparation method of the orthosilicate base fluorescent powder according to claim 3 or 5, it is characterised in that:Described contains
Magnesium ion Mg2+Compound include magnesia, magnesium hydroxide, magnesium carbonate, basic magnesium carbonate, magnesium nitrate in one kind;Described
Contain lithium ion Li+Compound include lithium carbonate, lithium hydroxide, lithium nitrate in one kind;Described contains europium ion Eu3+'s
Compound is one kind in europium oxide, europium nitrate.
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CN108913138A (en) * | 2018-08-10 | 2018-11-30 | 河南科技学院 | A kind of Eu3+Silicate-base red fluorescence powder of activation and preparation method thereof |
CN109705864A (en) * | 2018-11-23 | 2019-05-03 | 长春理工大学 | A kind of red fluorescence powder and preparation method thereof that luminous efficiency is high |
CN116120922A (en) * | 2023-02-17 | 2023-05-16 | 山东大学 | Eu (Eu) 2+ Silicate doped fluorescent material and preparation method and application thereof |
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CN105694870A (en) * | 2016-03-17 | 2016-06-22 | 常州工程职业技术学院 | Eu<3+> activated magnesium and sodium orthosilicate red fluorescent powder as well as preparation method and application thereof |
CN106085421A (en) * | 2016-06-06 | 2016-11-09 | 常州工程职业技术学院 | A kind of Eu3+positive magnesium silicate potassium fluorescent material activated and its preparation method and application |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108913138A (en) * | 2018-08-10 | 2018-11-30 | 河南科技学院 | A kind of Eu3+Silicate-base red fluorescence powder of activation and preparation method thereof |
CN108913138B (en) * | 2018-08-10 | 2021-06-04 | 河南科技学院 | Eu (Eu)3+Activated silicate-based red phosphor and method of making same |
CN109705864A (en) * | 2018-11-23 | 2019-05-03 | 长春理工大学 | A kind of red fluorescence powder and preparation method thereof that luminous efficiency is high |
CN116120922A (en) * | 2023-02-17 | 2023-05-16 | 山东大学 | Eu (Eu) 2+ Silicate doped fluorescent material and preparation method and application thereof |
CN116120922B (en) * | 2023-02-17 | 2024-01-30 | 山东大学 | Eu (Eu) 2+ Silicate doped fluorescent material and preparation method and application thereof |
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