CN108822842A - A kind of red strontium magnesium phosphate fluorescent and its preparation method and application - Google Patents
A kind of red strontium magnesium phosphate fluorescent and its preparation method and application Download PDFInfo
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- CN108822842A CN108822842A CN201810559802.4A CN201810559802A CN108822842A CN 108822842 A CN108822842 A CN 108822842A CN 201810559802 A CN201810559802 A CN 201810559802A CN 108822842 A CN108822842 A CN 108822842A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- BTEPQKGGXUMBRS-UHFFFAOYSA-K magnesium;strontium;phosphate Chemical compound [Mg+2].[Sr+2].[O-]P([O-])([O-])=O BTEPQKGGXUMBRS-UHFFFAOYSA-K 0.000 title claims abstract description 16
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 40
- 239000011777 magnesium Substances 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 13
- 238000004321 preservation Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910002538 Eu(NO3)3·6H2O Inorganic materials 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 3
- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims description 3
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 2
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Inorganic materials [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims 1
- 230000005284 excitation Effects 0.000 abstract description 11
- 238000001228 spectrum Methods 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 5
- 238000009877 rendering Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 238000010792 warming Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 28
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 15
- 239000010452 phosphate Substances 0.000 description 15
- 239000000843 powder Substances 0.000 description 15
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 7
- 238000000695 excitation spectrum Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 238000010791 quenching Methods 0.000 description 5
- 230000000171 quenching effect Effects 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 238000002284 excitation--emission spectrum Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- 238000006862 quantum yield reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910017677 NH4H2 Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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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
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7737—Phosphates
- C09K11/7738—Phosphates with alkaline earth metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
A kind of red strontium magnesium phosphate fluorescent and its preparation method and application, which is Sr19(1‑x)Eu19xMg2(PO4)14, according to each element molar ratio Sr in raw material:Eu:Mg=19 (1-x):19x:2；Mg:P=1:7 weigh raw material, after mixing under reducing atmosphere, are first heated to 900 DEG C of heat preservation 4h, then be warming up to 1200 DEG C of heat preservation 6h, cool to room temperature with the furnace.Advantage is：Eu2+After ion doping, Sr19Mg2(PO4)14；Eu2+Launch wavelength can be obtained at 400nm in the feux rouges of 625nm in excitation wavelength, provide red spectrum needed for high-color rendering in semiconductor lighting, and there is high luminous efficiency, good thermal stability and chemical stability.Product preparation method is simple, and synthesis condition is mild, is suitable for producing in enormous quantities, great industry application value.
Description
Technical field
The present invention relates to a kind of red strontium magnesium phosphate fluorescent and its preparation method and application, in particular to a kind of use
The red phosphate fluorescent and its preparation method and application of luminescence generated by light in semiconductor lighting.
Background technique
WLEDs lamp has unique advantage in terms of energy-saving and environmental protection, service life, is that section is advocated and participated in jointly in the whole world
Energy, environmentally friendly development need, in addition, LED light is due to pollutants such as its is unleaded, mercury, it is real environment-friendly products.
WLEDs white light source can be obtained in conjunction with red, green, blue three fluorescence material by (close) ultraviolet chip, and
Colour rendering index is high, colour temperature is low simultaneously, in order to improve the colour rendering and stability of final WLEDs, it is desirable that the excitation of (close) ultraviolet chip
Fluorescent material have the Wavelength matched property of good chip, stability and higher luminous efficiency.Therefore, it needs to research and develop novel
Efficient and good stability luminescent material.
Currently, can have high efficiency, the red illuminating material of excellent thermal stability few by (close) burst of ultraviolel
There is registration.Wherein the red fluorescence material representative of better performances is Y2O2S:Eu3+, but they are due in sulfate preparation process
There is the by-product of sulfide to generate, pollution will cause to environment, and within specified temperatures, chemical stability is poor, direct shadow
Ring light conversion efficiency, Y2O2S:Eu3+Stability need to be further increased.In addition, Eu3+F-f transition absorption belong to threadiness
Absorption peak, there is some difference with the emission peak matching of current commercial LED chip (365nm~410nm), seriously affects device
Light conversion efficiency.Nitride phosphor is since with unique excitation spectrum, (excites scope covers ultraviolet, near ultraviolet, blue light
Even green light) and the excellent characteristics of luminescence, it develops and receives the very big concern of scientific circles and industrial circle.Nitride is glimmering
Luminescent material luminous efficiency with higher, good Wavelength matched property and stability in recent years by people's extensive concern,
However nitride fluorescent material preparation process needs the harshnesses such as high temperature (1600 degree of >), high pressure (0.1~10MPa), atmosphere protection
Condition significantly limits the extensive use and popularization of the fluorescent powder.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of Spectral matching is good, luminous efficiency is high, preparation method is easy
And the red strontium magnesium phosphate fluorescent and its preparation method and application that synthesis temperature is low.
The technical solution of the invention is as follows：
A kind of red strontium magnesium phosphate fluorescent, chemical constitution formula Sr19(1-x)Eu19xMg2(PO4)14, wherein 0.001≤x
≤0.09。
A kind of preparation method of red strontium magnesium phosphate fluorescent, includes the following steps：
1) according to chemical constitution formula Sr19(1-x)Eu19xMg2(PO4)14, according to each element molar ratio Sr in raw material:Eu:Mg=19
(1-x):19x:2；Mg:P=1:7 weigh raw material, wherein 0.001≤x≤0.09, wherein the raw material includes：
The oxide (SrO) that contains Sr can be converted into the compound of the oxide as the source Sr；
The oxide (MgO) that contains Mg can be converted into the compound of the oxide as the source Mg；
Contain the simple substance, oxide, nitrate of Eu as the source Eu；
The compound of the oxide that contains P or the oxide that can be converted into P is as the source P；
2) above-mentioned raw materials are mixed to get mixture, under reducing atmosphere, mixture are first heated to 900 DEG C of heat preservation 4h, then rise
Temperature cools to room temperature with the furnace to 1200 DEG C of heat preservation 6h.
The source Sr is SrO, SrCO3、Sr(NO3)2·4H2O、SrC2O4Or Sr (CH3COO)2。
The source Mg is MgO, MgCO3、4MgCO3·Mg(OH)2·5H2O。
The source P is (NH4)2HPO4、NH4H2PO4、H3PO4Or P2O5。
The source Eu is Eu simple substance, Eu2O3Or Eu (NO3)3·6H2O。
Reducing atmosphere described in step 2 is one or more of nitrogen, hydrogen or ammonia mixed atmosphere.
It is a kind of red strontium magnesium phosphate fluorescent production white light LEDs in application.
The beneficial effects of the invention are as follows：
(1) phosphate material with pyrophosphorite (Whitlockite-type) crystal structure is since synthesis temperature is lower, object
The advantages that Physicochemical stability is good is widely used in the numerous areas such as laser material, biomaterial and luminescent material.This hair
Bright first passage adjusts experiment condition and raw material proportioning has synthesized Eu2+The red fluorescence material Sr of ion doping19Mg2
(PO4)14:Eu2+.The red phosphate fluorescent belongs to pyrophosphorite crystal structure, space group R-3m.Eu2+Ion doping
Afterwards, Sr19Mg2(PO4)14；Eu2+Launch wavelength can be obtained at 400nm in the feux rouges of 625nm in excitation wavelength, provide half
Red spectrum needed for high-color rendering in conductor illumination, while having high luminous efficiency, good thermal stability and chemistry steady
It is qualitative.Product preparation method is simple, can synthesize under normal pressure, and calcination temperature is lower, is suitable for producing in enormous quantities, great industry
Application value.
(2) by the ratio of the Sr and Eu that adjust, Eu is prepared in a reducing atmosphere2+Fluorescent material, in 365nm to 410nm
Range has wider excites scope, can have preferable matching near ultraviolet LED chip, and exist in excitation wavelength
Launch wavelength can be obtained at 400nm in the feux rouges of 625nm.It is obtained by adjusting doping ratio parameter setting with can be convenient simultaneously
To the scheme for being applicable in different product, there is very strong applicability, the Sr under 400nm shooting condition18.81Eu0.19Mg2(PO4)14Hair
Brightness can achieve the 68.3% of commercial powder light emission luminance, and compared to commercial powder, Sr19Mg2(PO4)14Red phosphate
Fluorescent material have many advantages, such as it is cheap, production prepare it is simple, it is potential as a kind of novel red luminescent material.
Detailed description of the invention
Below in conjunction with figure embodiment, the invention will be further described：
Fig. 1 is the XRD diffracting spectrum of red phosphate fluorescent in the embodiment of the present invention 1；
Fig. 2 is the exciting light spectrogram and launching light spectrogram of red phosphate fluorescent in the embodiment of the present invention 1；
Fig. 3 is the thermal quenching curve graph of red phosphate fluorescent in the embodiment of the present invention 1；
Fig. 4 is the XRD diffracting spectrum of red phosphate fluorescent in the embodiment of the present invention 2；
Fig. 5 is the exciting light spectrogram and launching light spectrogram of red phosphate fluorescent in the embodiment of the present invention 2；
Fig. 6 is the thermal quenching curve graph of red phosphate fluorescent in the embodiment of the present invention 2；
Fig. 7 is the XRD diffracting spectrum of red phosphate fluorescent in the embodiment of the present invention 3；
Fig. 8 is the exciting light spectrogram and launching light spectrogram of red phosphate fluorescent in the embodiment of the present invention 3；
Fig. 9 is the thermal quenching curve graph of red phosphate fluorescent in the embodiment of the present invention 3；
Figure 10 is red phosphate fluorescent and current commercial red fluorescence powder Y in the embodiment of the present invention 22O2S:Eu3+Transmitting
Intensity compares.
Specific embodiment
In order to further appreciate that the present invention, the preferred embodiments of the invention are described below with reference to embodiment, but
It is it should be appreciated that these descriptions are intended merely to further illustrate the features and advantages of the present invention, rather than want to right of the present invention
The limitation asked.
Embodiment 1
(1) according to chemical formula Sr19Mg2(PO4)14：0.005Eu2+(Sr18.905Eu0.095Mg2(PO4)14) composition weigh 0.9153g
SrCO3, 0.0264g MgO, 0.6063g (NH4)2HPO4With 0.0054g Eu2O3, 30min is ground, raw material is uniformly mixed and obtains
Mixed powder；
(2) mixed powder is put into corundum crucible, is put into tube-type atmosphere furnace, be passed through the N that mixing reducing gas flows2/
H2In (its volume ratio be 9/1) reducing atmosphere, 900 DEG C of heat preservation 4h are risen to the heating rate of 5 DEG C/min, then again with 5 DEG C/
The heating rate of min rises to 1200 DEG C, keeps the temperature 6h, cooled to room temperature after being then down to 500 DEG C with the rate of 5 DEG C/min,
Obtained powder is taken out to grind and obtains required phosphor material powder at powder.
As shown, Fig. 1 shows 1 gained sample Sr of embodiment18.905Eu0.095Mg2(PO4)14XRD spectrum, basic structure
For pyrophosphorite crystal structure, there is R-3m space group.
Fig. 2 shows the excitation spectrum and emission spectrum of gained fluorescent material in embodiment 1；As can be seen that the fluorescent material exists
625nm monitors lower excitation spectrum and shows as the 300 broadband excitation peaks for arriving 450nm range, and has near 400nm and stronger to swash
Hair, in terms of illustrating that it can be applied to the white light LEDs of UV LED chip excitation.Under 400nm excitation, sample shows feux rouges
Transmitting, range extend near 750nm from 550nm, and transmitting peak wavelength is located near 625nm, can be near ultraviolet LED chip
There is preferable matching.
Fig. 3 gives the thermal quenching spectrum of gained fluorescent material in embodiment 1, the results showed that, as the temperature gradually increases, sample
The emission peak of product has certain decrease, and when temperature drops to 413K (140 DEG C), emissive porwer, which remains unchanged, keeps initial strength
36.27%.
By testing the discovery of its quantum efficiency, the Sr18.905Eu0.095Mg2(PO4)14Phosphor material powder absolute quantum yield can reach
To 75%.
Embodiment 2
(1) according to chemical formula Sr19Mg2(PO4)14:0.01Eu2+(Sr18.81Eu0.19Mg2(PO4)14) composition weigh 1.7465g Sr
(NO3)2·4H2O, 0.0636g 4MgCO3·Mg(OH)2·5H2O, 0.4490g H3PO4With 0.0109g Eu2O3, grinding
45min is uniformly mixed raw material；
(2) mixed powder is put into corundum crucible, is put into tube-type atmosphere furnace, be passed through the N that mixing reducing gas flows2/
H2In mixed atmosphere (nitrogen and hydrogen volume ratio be 9/1) reducing atmosphere, 900 DEG C of heat preservations are risen to the heating rate of 5 DEG C/min
Then 4h rises to 1200 DEG C again with the heating rate of 5 DEG C/min, 6h is kept the temperature, after being then down to 500 DEG C with the rate of 5 DEG C/min
Obtained powder is taken out grinding and obtains required phosphor material powder at powder by cooled to room temperature.Fig. 4 shows implementation
2 gained sample Sr of example18.81Eu0.19Mg2(PO4)14XRD spectrum, basic structure be pyrophosphorite crystal structure, have R-3m
Space group.Fig. 5 shows the excitation spectrum and emission spectrum of gained fluorescent material in embodiment 2；It can be seen that the fluorescent material
Excitation spectrum shows as 300 and arrives the broadband excitation peaks of 450nm range under 625nm monitoring, and has near 400nm stronger
Excitation, can there is preferable matching near ultraviolet LED chip.Under 400nm monitoring, sample shows red emission, range
It is extended near 750nm from 550nm, transmitting peak wavelength is located near 625nm.Fig. 6 gives gained phosphor in embodiment 2
The thermal quenching spectrum of material, the results showed that, as the temperature gradually increases, the emission peak of sample has certain decrease, at a temperature of
When dropping to 413K (140 DEG C), emissive porwer, which remains unchanged, keeps the 40.94% of initial strength.By testing the discovery of its quantum efficiency,
The sample absolute quantum yield can achieve 79%.
Embodiment 3
(1) according to chemical formula Sr19Mg2(PO4)14:0.02Eu2+(Sr18.62Eu0.38Mg2(PO4)14) composition weigh 0.6290g
SrO, 0.0263g MgO, 0.5250g NH4H2PO4With 0.0552g Eu (NO3)3·6H2O grinds 60min, keeps raw material mixing equal
It is even；
(2) mixed powder is put into corundum crucible, is put into tube-type atmosphere furnace, be passed through the N that mixing reducing gas flows2/
H2In (its volume ratio be 9/1) reducing atmosphere, 900 DEG C of heat preservation 4h are risen to the heating rate of 5 DEG C/min, then again with 5 DEG C/
The heating rate of min rises to 1200 DEG C, keeps the temperature 6h, cooled to room temperature after being then down to 500 DEG C with the rate of 5 DEG C/min,
Obtained powder is taken out to grind and obtains required phosphor material powder at powder.Fig. 7 shows 3 gained sample of embodiment
Sr18.62Eu0.38Mg2(PO4)14XRD spectrum, basic structure be pyrophosphorite crystal structure, have R-3m space group.Fig. 8
Show the excitation spectrum and emission spectrum of gained fluorescent material in embodiment 3；As can be seen that the fluorescent material is supervised in 625nm
It controls lower excitation spectrum and shows as 300 and arrive the broadband excitation peak of 450nm range, and have stronger excitation near 400nm, it can be with
There is preferable matching near ultraviolet LED chip.Under 400nm monitoring, sample shows red emission, and range is prolonged from 550nm
It reaches near 750nm, transmitting peak wavelength is located near 625nm.The heat that Fig. 9 gives gained fluorescent material in embodiment 3 is sudden
Go out spectrum, the results showed that, as the temperature gradually increases, the emission peak of sample has certain decrease, when temperature drops to 413K
When (140 DEG C), emissive porwer, which remains unchanged, keeps the 46.43% of initial strength.By testing the discovery of its quantum efficiency, the sample is exhausted
74% can achieve to quantum yield.
Figure 10 is red phosphate fluorescent and the commercial phosphor emission intensity ratio of existing market circulation in present example 2
Compared with.As can be seen that the Sr under 400nm shooting condition18.81Eu0.19Mg2(PO4)14Light emission luminance can achieve commercial powder luminance
The 68.3% of degree, potential novel red luminescent material a kind of.It is handled by subsequent technique, luminous intensity is expected into one
Step improves.
The above is only specific embodiments of the present invention, are not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of red strontium magnesium phosphate fluorescent, it is characterized in that：Chemical constitution formula Sr19(1-x)Eu19xMg2(PO4)14, wherein
0.001≤x≤0.09。
2. a kind of preparation method of red strontium magnesium phosphate fluorescent, it is characterized in that：Include the following steps：
1) according to chemical constitution formula Sr19(1-x)Eu19xMg2(PO4)14, according to each element molar ratio Sr in raw material:Eu:Mg=19 (1-
x):19x:2；Mg:P=1:7 weigh raw material, wherein 0.001≤x≤0.09, wherein the raw material includes：
The oxide (SrO) that contains Sr can be converted into the compound of the oxide as the source Sr；
The oxide (MgO) that contains Mg can be converted into the compound of the oxide as the source Mg；
Contain the simple substance, oxide, nitrate of Eu as the source Eu；
The compound of the oxide that contains P or the oxide that can be converted into P is as the source P；
2) above-mentioned raw materials are mixed to get mixture, under reducing atmosphere, mixture are first heated to 900 DEG C of heat preservation 4h, then rise
Temperature cools to room temperature with the furnace to 1200 DEG C of heat preservation 6h.
3. the preparation method of red strontium magnesium phosphate fluorescent according to claim 2, it is characterized in that：The source Sr is
SrO、SrCO3、Sr(NO3)2·4H2O、SrC2O4Or Sr (CH3COO)2。
4. the preparation method of red strontium magnesium phosphate fluorescent according to claim 2, it is characterized in that：The source Mg is
MgO、MgCO3、4MgCO3·Mg(OH)2·5H2O。
5. the preparation method of red strontium magnesium phosphate fluorescent according to claim 2, it is characterized in that：The source P is
(NH4)2HPO4、NH4H2PO4、H3PO4Or P2O5。
6. the preparation method of red strontium magnesium phosphate fluorescent according to claim 2, it is characterized in that：The source Eu is
Eu simple substance, Eu2O3Or Eu (NO3)3·6H2O。
7. the preparation method of red strontium magnesium phosphate fluorescent according to claim 2, it is characterized in that：Institute in step 2
Stating reducing atmosphere is one or more of nitrogen, hydrogen or ammonia mixed atmosphere.
8. a kind of application of red strontium magnesium phosphate fluorescent as described in weighing and require 1 in production white light LEDs.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111778021A (en) * | 2020-07-14 | 2020-10-16 | 新疆师范大学 | High-luminescence thermal-stability bluish violet luminescent material and preparation method and application thereof |
| CN112159659A (en) * | 2020-09-15 | 2021-01-01 | 上海应用技术大学 | Single-phase full-spectrum fluorescent powder for high-quality healthy lighting LED and preparation method and application thereof |
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| CN107474841A (en) * | 2017-07-10 | 2017-12-15 | 渤海大学 | A kind of red bismuth phosphate fluorescent material and its preparation method and application |
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| CN107474841A (en) * | 2017-07-10 | 2017-12-15 | 渤海大学 | A kind of red bismuth phosphate fluorescent material and its preparation method and application |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111778021A (en) * | 2020-07-14 | 2020-10-16 | 新疆师范大学 | High-luminescence thermal-stability bluish violet luminescent material and preparation method and application thereof |
| CN111778021B (en) * | 2020-07-14 | 2022-11-04 | 新疆师范大学 | High-luminescence thermal-stability bluish violet luminescent material and preparation method and application thereof |
| CN112159659A (en) * | 2020-09-15 | 2021-01-01 | 上海应用技术大学 | Single-phase full-spectrum fluorescent powder for high-quality healthy lighting LED and preparation method and application thereof |
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| CN108822842B (en) | 2021-06-11 |
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