CN105419798A - Preparation method and application of orange-red antimonate fluorescent material - Google Patents

Preparation method and application of orange-red antimonate fluorescent material Download PDF

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CN105419798A
CN105419798A CN201510979018.5A CN201510979018A CN105419798A CN 105419798 A CN105419798 A CN 105419798A CN 201510979018 A CN201510979018 A CN 201510979018A CN 105419798 A CN105419798 A CN 105419798A
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compound
preparation
orange red
antimonate
europium
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CN105419798B (en
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乔学斌
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Xuzhou Bochuang Construction Development Group Co ltd
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Jiangsu Normal University
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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

Abstract

The invention discloses a preparation method and an application of an orange-red antimonate fluorescent material and belongs to the field of inorganic light-emitting materials. A chemical general formula of the orange-red antimonate fluorescent material is Ca<5-5x>Eu<5x>Sb<5>O<17>, wherein X is the molar percentage of doped Eu<3+>, 0.001 <= x <= 0.15. The preparation method mainly includes a high-temperature solid-phase method and a chemical synthetic method. The orange-red antimonate fluorescent powder can be excited by means of light being 200-450 nm in wavelength to emit orange-red light being 612 nm in main wavelength. The raw materials in the preparation method are low in cost and easy to obtain. The preparation method is simple and is easy to carry out. The fluorescent material is stable in chemical properties of a substrate, is excellent in light-emitting performance and has wide application prospect in the field of LED illumination.

Description

A kind of preparation method of orange red antimonate luminescent materials and application
Technical field
The present invention relates to a kind of preparation method and application of orange red antimonate luminescent materials, particularly the preparation method of the orange red stibnate phosphor material powder of the ultraviolet of a kind of wavelength in 200 ~ 450 nanometer range, near ultraviolet and excited by visible light and application thereof.
Background technology
Since entering the new millennium; how save energy and protection of the environment are the major issues that people face always; in illumination field; white light LEDs has better energy-saving effect relative to traditional incandescent light; and stable luminescent property, long service life, thus greatly reduce the loss to the energy; be described as the green energy resource of new millennium by people, and cause the extensive research of people.
Current most popular white light LEDs, mainly with the fluorescent material of GaN base chip collocation YAG:Ce, to launch by exciting YAG:Ce that gold-tinted and blue light realize.But owing to lacking red color light component in its light source, cause its colour rendering index lower, color reducibility is poor, the colder tone of tone, make in numerous lamp red fluorescence powders, really can be practical and few, the red fluorescence powder therefore near ultraviolet to blue light range with efficient absorption becomes the focus of research both at home and abroad at present.
Stibnate is with its abundant kind and stable physicochemical property, and the substrate material of fluorescent material is widely used in by people, this is mainly because stibnate has good optical absorption band, by the transmission ofenergy of absorption to the rare earth ion be entrained in stibnate matrix, thus luminous effect can be reached after high-octane optical excitation.Europium doped ion Eu in stibnate matrix 3+the red fluorescence powder prepared has good colouring intensity and pure colourity, and this point is at the Ca of the structure of double perovskite of people's reports such as XinLin 2laSbO 6: there is good introduction in Eu red fluorescence powder.This report basis we have studied the orange red luminescent material of calcium antimonate, and this phosphor material powder was not yet reported at present.
Summary of the invention
The object of the invention is to the deficiency overcoming existing lamp phosphor technology, there is provided that a kind of preparation technology is simple, performance efficiency and the emission peak metaantimmonic acid alkali orange red fluorescent powder material that can be able to regulate between 550 ~ 650, make it under the exciting of ultraviolet and visible ray, launch the orange red light of efficient stable.
For achieving the above object, the technical solution used in the present invention is: provide a kind of orange red antimonate luminescent materials, and its chemical general formula is Ca 5-5xeu 5xsb 5o 17, wherein x is Eu 3+the molecular fraction of doping, 0.001≤x≤0.15; Described stibnate based luminescent material has very strong response to the light in 200 ~ 450 nanometer range, can launch the orange red light of predominant wavelength in 612 nanometers.
A preparation method for orange red antimonate luminescent materials, adopts high temperature solid-state method, it is characterized in that comprising the steps:
(1) by chemical formula Ca 5-5xeu 5xsb 5o 17in the stoichiometric ratio of each element, wherein 0.001≤x≤0.15, takes respectively containing calcium ion Ca 2+compound, containing europium ion Eu 3+compound, containing antimony ion Sb 3+compound, grind and mix, obtaining mixture;
(2) mixture that step (1) obtains is placed in retort furnace, precalcining in air atmosphere, precalcining temperature is 300 ~ 700 DEG C, and the precalcining time is 2 ~ 16 hours;
(3) by mixture naturally cooling that step (2) obtains, to grind and after mixing, again be placed in retort furnace, calcine in air atmosphere, calcining temperature is 700 ~ 1100 DEG C, calcination time is 1 ~ 12 hour, naturally cools to room temperature, obtains a kind of stibnate luminescent material can launching orange red light under ultraviolet, near ultraviolet excitation after grinding evenly.
Further, the precalcining temperature of step (2) is 350 ~ 650 DEG C, and the precalcining time is 3 ~ 12 hours.
Further, the calcining temperature of step (3) is 750 ~ 1000 DEG C, and calcination time is 2 ~ 9 hours.
Further, calcium ions Ca 2+compound be one in calcium carbonate, calcium chloride, nitrocalcite, calcium hydroxide, calcium oxide; Described contains europium ion Eu 3+compound be one in europium sesquioxide, europium nitrate, Europium trichloride; Described contains antimony ion Sb 3+compound be one in antimonous oxide, antimony chloride or nitric acid antimony.
A preparation method for orange red antimonate luminescent materials, adopts chemical synthesis, comprises the steps:
(1) by chemical formula Ca 5-5xeu 5xsb 5o 17in the stoichiometric ratio of each element, wherein 0.001≤x≤0.15, takes respectively containing calcium ion Ca 2+compound, containing europium ion Eu 3+compound, containing antimony ion Sb 3+compound, they are used dust technology and deionized water dissolving respectively, then add complexing agent citric acid or oxalic acid respectively by 0.5 ~ 2.0wt% of each reactant quality, obtain the mixing solutions of each raw material;
(2) each mixing solutions that step (1) obtains slowly is mixed, then under the temperature condition of 50 ~ 80 DEG C stir 1 ~ 2 hour, leave standstill, dry after obtain bulk presoma;
(3) presoma that step (2) obtains is placed in retort furnace to calcine, calcining temperature is 500 ~ 950 DEG C, calcination time is 2 ~ 10 hours, naturally cools to room temperature, obtains a kind of stibnate luminescent material can launching orange red light under ultraviolet, near ultraviolet excitation after grinding evenly.
Further, the calcining temperature of step (3) is 600 ~ 900 DEG C, and calcination time is 3 ~ 9 hours.
Further, described calcium ions Ca 2+compound be one in calcium carbonate, calcium chloride, nitrocalcite, calcium hydroxide, calcium oxide; Described contains europium ion Eu 3+compound be one in europium sesquioxide, europium nitrate, Europium trichloride; Described contains antimony ion Sb 3+compound be one in antimonous oxide, antimony chloride or nitric acid antimony.A kind of orange red antimonate luminescent materials is applied to the adjustment with photoluminescence colourity in various luminouslighting material.
Compared with prior art, tool of the present invention has the following advantages: stibnate base fluorescent powder provided by the invention has abundant kind, has wider absorption band and higher light transmission, and relative to other fluorescent material, if sulfide, halogenide are the material of base, its environmental-protecting performance is better.Stibnate base fluorescent powder provided by the invention, the process of preparation is simple to operation, reproducible, and does not need reducing atmosphere to protect in whole process, because this reducing energy consumption, and less demanding for equipment, also greatly reduce production cost.Stibnate base fluorescent powder designed by the present invention, by the optical excitation of wavelength in 200 ~ 450 nanometer range, can launch the orange red light of 550-650 nanometer range, can be applied in novel white light LEDs.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 1 prepares sample Ca 4.95eu 0.05sb 5o 17x-ray powder diffraction pattern.
Fig. 2 is that the embodiment of the present invention 1 prepares sample Ca 4.95eu 0.05sb 5o 17sEM(scanning electronic microscope) collection of illustrative plates.
Fig. 3 is that the embodiment of the present invention 1 prepares sample Ca 4.95eu 0.05sb 5o 17exciting light spectrogram under 612 nano wave length monitorings.
Fig. 4 is that the embodiment of the present invention 1 prepares sample Ca 4.95eu 0.05sb 5o 17luminescent spectrum figure under 396 nano wave lengths excite.
Fig. 5 is that the embodiment of the present invention 1 prepares sample Ca 4.95eu 0.05sb 5o 17decay of luminescence curve under 612 nano wave length monitorings.
Fig. 6 is that the embodiment of the present invention 5 prepares sample Ca 4.25eu 0.75sb 5o 17x-ray powder diffraction pattern.
Fig. 7 is that the embodiment of the present invention 5 prepares sample Ca 4.25eu 0.75sb 5o 17sEM(scanning electronic microscope) collection of illustrative plates.
Fig. 8 is that the embodiment of the present invention 5 prepares sample Ca 4.25eu 0.75sb 5o 17exciting light spectrogram under 612 nano wave length monitorings.
Fig. 9 is that the embodiment of the present invention 5 prepares sample Ca 4.25eu 0.75sb 5o 17luminescent spectrum figure under 396 nano wave lengths excite.
Figure 10 is that the embodiment of the present invention 5 prepares sample Ca 4.25eu 0.75sb 5o 17decay of luminescence curve under 612 nano wave length monitorings.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Embodiment 1:
Preparation Ca 4.95eu 0.05sb 5o 17
According to chemical formula Ca 4.95eu 0.05sb 5o 17in the stoichiometric ratio of each element, take calcium carbonate CaCO respectively 3: 0.9900 gram, europium sesquioxide Eu 2o 3: 0.0352 gram, antimonous oxide Sb 2o 3: 1.4575 grams, to grind in agate mortar and after mixing, select air atmosphere precalcining 3 hours at 650 DEG C in retort furnace, be then chilled to room temperature, take out sample; Again that abundant for compound mixed grinding is even, among air atmosphere, calcine 2 hours at 1000 DEG C, be cooled to room temperature, take out rear and abundant grinding and namely obtain pulverous stibnate material can launching orange red light.
See accompanying drawing 1, it is the X-ray powder diffraction pattern that the present embodiment technical scheme prepares sample, and XRD test result shows, and occur without other assorted peak in figure, the sample obtained by explanation is single-phase material;
See accompanying drawing 2, it is the SEM(scanning electronic microscope by sample prepared by the present embodiment technical scheme) collection of illustrative plates; As can be seen from the figure, gained sample good crystallinity, Granular composite is even, and its median size is 3.02 microns;
See accompanying drawing 3, it is the exciting light spectrogram of sample under 612 nano wave length monitorings prepared by the present embodiment technical scheme; As seen from the figure, this material well can be excited by the light of wavelength in 200 ~ 450 nanometer range;
See accompanying drawing 4, it is the luminescent spectrum figure of sample under 396 nano wave lengths excite prepared by the present embodiment technical scheme, and as seen from the figure, this material can launch the orange red light of predominant wavelength at 612 nm;
See accompanying drawing 5, it is the decay of luminescence curve of sample under 612 nano wave length monitorings prepared by the present embodiment technical scheme, and can be calculated fall time is 2.39 milliseconds.
Embodiment 2:
Preparation Ca 4.9eu 0.1sb 5o 17
According to chemical formula Ca 4.9eu 0.1sb 5o 17in the stoichiometric ratio of each element, take nitrocalcite Ca (NO respectively 3) 24H 2o:2.3143 gram, europium sesquioxide Eu 2o 3: 0.0704 gram, antimonous oxide Sb 2o 3: 1.4575 grams, to grind in agate mortar and after mixing, select air atmosphere precalcining 8 hours at 450 DEG C in retort furnace, be then chilled to room temperature, take out sample; Again that abundant for compound mixed grinding is even, among air atmosphere, calcine 6 hours at 850 DEG C, be cooled to room temperature, take out rear and abundant grinding and namely obtain pulverous stibnate material can launching orange red light.
Its primary structure pattern, excitation spectrum, emmission spectrum and extinction curve are similar to embodiment 1.
Embodiment 3:
Preparation Ca 4.85eu 0.15sb 5o 17
According to chemical formula Ca 4.85eu 0.15sb 5o 17in the stoichiometric ratio of each element, take calcium oxide CaO:0.5439 gram respectively, Europium trichloride EuCl 36H 2o:0.1099 gram, antimonous oxide Sb 2o 3: 1.4575 grams, to grind in agate mortar and after mixing, select air atmosphere precalcining 6 hours at 550 DEG C in retort furnace, be then chilled to room temperature, take out sample; Again that abundant for compound mixed grinding is even, among air atmosphere, calcine 4 hours at 950 DEG C, be cooled to room temperature, take out rear and abundant grinding and namely obtain pulverous stibnate material can launching orange red light;
Its primary structure pattern, excitation spectrum, emmission spectrum and extinction curve are similar to embodiment 1.
Embodiment 4:
Preparation Ca 4.8eu 0.2sb 5o 17
According to chemical formula Ca 4.8eu 0.2sb 5o 17in the stoichiometric ratio of each element, take calcium hydroxide Ca (OH) respectively 2: 0.7113 gram, europium nitrate Eu (NO 3) 36H 2o:0.1352 gram, antimonous oxide Sb 2o 3: 1.4575 grams, to grind in agate mortar and after mixing, select air atmosphere precalcining 12 hours at 350 DEG C in retort furnace, be then chilled to room temperature, take out sample; Again that abundant for compound mixed grinding is even, among air atmosphere, calcine 9 hours at 750 DEG C, be cooled to room temperature, take out rear and abundant grinding and namely obtain pulverous stibnate material can launching orange red light;
Its primary structure pattern, excitation spectrum, emmission spectrum and extinction curve are similar to embodiment 1.
Embodiment 5:
Preparation Ca 4.25eu 0.75sb 5o 17
According to chemical formula Ca 4.25eu 0.75sb 5o 17in the stoichiometric ratio of each element, take calcium chloride CaCl respectively 2: 0.9433 gram, Europium trichloride EuCl 36H 2o:0.5496 gram, antimony chloride SbCl 3: 2.8811 grams, and the citric acid of the 2.0wt% of above each raw material total mass; Use appropriate deionized water and nitric acid dissolve above-mentioned raw materials respectively, uniform stirring, until dissolve completely, and then carry out complexing with citric acid respectively, finally mixed by dissolution homogeneity good for above-mentioned complexing, be heated to 80 DEG C and stir 2 hours, standing, oven dry obtains bulk presoma; Precursor is placed in retort furnace calcine, calcining temperature is 900 DEG C, and calcination time is 3 hours, is cooled to room temperature, takes out rear and abundant grinding and namely obtains pulverous stibnate material can launching orange red light.
See accompanying drawing 6, it is the X-ray powder diffraction pattern that the present embodiment technical scheme prepares sample, and XRD test result shows, and occur without other assorted peak in figure, the sample obtained by explanation is single-phase material;
See accompanying drawing 7, it is the SEM(scanning electronic microscope by sample prepared by the present embodiment technical scheme) collection of illustrative plates; As can be seen from the figure, gained sample particle is uniformly dispersed, and its median size is 2.43 microns;
See accompanying drawing 8, it is the exciting light spectrogram of sample under 612 nano wave length monitorings prepared by the present embodiment technical scheme; As seen from the figure, this material well can be excited by the light of wavelength in 200 ~ 450 nanometer range;
See accompanying drawing 9, it is the luminescent spectrum figure of sample under 396 nano wave lengths excite prepared by the present embodiment technical scheme, and as seen from the figure, this material can launch the orange red light of predominant wavelength at 612 nm;
See accompanying drawing 10, it is the decay of luminescence curve of sample under 612 nano wave length monitorings prepared by the present embodiment technical scheme, and can be calculated fall time is 3.23 milliseconds.
Embodiment 6:
Preparation Ca 4.5eu 0.5sb 5o 17
According to chemical formula Ca 4.5eu 0.5sb 5o 17in the stoichiometric ratio of each element, take nitrocalcite Ca (NO respectively 3) 24H 2o:2.1253 gram, Europium trichloride EuCl 36H 2o:0.3664 gram, antimony chloride SbCl 3: 2.8811 grams, and the citric acid of the 2.0wt% of above each raw material total mass; Use appropriate deionized water and nitric acid dissolve above-mentioned raw materials respectively, uniform stirring, until dissolve completely, then complexing is being carried out with citric acid respectively, finally mixed by dissolution homogeneity good for above-mentioned complexing, be heated to 80 DEG C and stir 2 hours, standing, oven dry obtains bulk presoma; Precursor is placed in retort furnace calcine, calcining temperature is 800 DEG C, and calcination time is 5 hours, is cooled to room temperature, takes out rear and abundant grinding and namely obtains pulverous stibnate material can launching orange red light.
Its primary structure pattern, excitation spectrum, emmission spectrum and extinction curve are similar to embodiment 5.
Embodiment 7:
Preparation Ca 4.995eu 0.005sb 5o 17
According to chemical formula Ca 4.995eu 0.005sb 5o 17in the stoichiometric ratio of each element, take calcium chloride CaCl respectively 2: 1.1087 grams, europium nitrate Eu (NO 3) 36H 2o:0.0033 gram, nitric acid antimony Sb (NO 3) 3: 2.1172 grams, and the citric acid of the 2.0wt% of above each raw material total mass; Use appropriate deionized water and nitric acid dissolve above-mentioned raw materials respectively, uniform stirring, until dissolve completely, then complexing is being carried out with citric acid respectively, finally mixed by dissolution homogeneity good for above-mentioned complexing, be heated to 80 DEG C and stir 2 hours, standing, oven dry obtains bulk presoma; Precursor is placed in retort furnace calcine, calcining temperature is 700 DEG C, and calcination time is 7 hours, is cooled to room temperature, takes out rear and abundant grinding and namely obtains pulverous stibnate material can launching orange red light.
Its primary structure pattern, excitation spectrum, emmission spectrum and extinction curve are similar to embodiment 5.
Embodiment 8
Preparation Ca 4.975eu 0.025sb 5o 17
According to chemical formula Ca 4.975eu 0.025sb 5o 17in the stoichiometric ratio of each element, take nitrocalcite Ca (NO respectively 3) 24H 2o:2.3497 gram, europium nitrate Eu (NO 3) 36H 2o:0.0169 gram, nitric acid antimony Sb (NO 3) 3: 2.1172 grams, and the citric acid of the 2.0wt% of above each raw material total mass; Use appropriate deionized water and nitric acid dissolve above-mentioned raw materials respectively, uniform stirring, until dissolve completely, then complexing is being carried out with citric acid respectively, finally mixed by dissolution homogeneity good for above-mentioned complexing, be heated to 80 DEG C and stir 2 hours, standing, oven dry obtains bulk presoma; Precursor is placed in retort furnace calcine, calcining temperature is 600 DEG C, and calcination time is 9 hours, is cooled to room temperature, takes out rear and abundant grinding and namely obtains pulverous stibnate material can launching orange red light.
Its primary structure pattern, excitation spectrum, emmission spectrum and extinction curve are similar to embodiment 5.

Claims (9)

1. an orange red antimonate luminescent materials, is characterized in that: its chemical general formula is Ca 5-5xeu 5xsb 5o 17, wherein x is Eu 3+the molecular fraction of doping, 0.001≤x≤0.15.
2. a preparation method for orange red antimonate luminescent materials, adopts high temperature solid-state method, it is characterized in that comprising the steps:
(1) by chemical formula Ca 5-5xeu 5xsb 5o 17in the stoichiometric ratio of each element, wherein 0.001≤x≤0.15, takes respectively containing calcium ion Ca 2+compound, containing europium ion Eu 3+compound, containing antimony ion Sb 3+compound, grind and mix, obtaining mixture;
(2) mixture that step (1) obtains is placed in retort furnace, precalcining in air atmosphere, precalcining temperature is 300 ~ 700 DEG C, and the precalcining time is 2 ~ 16 hours;
(3) by mixture naturally cooling that step (2) obtains, to grind and after mixing, again be placed in retort furnace, calcine in air atmosphere, calcining temperature is 700 ~ 1100 DEG C, calcination time is 1 ~ 12 hour, naturally cools to room temperature, obtains a kind of stibnate luminescent material can launching orange red light under ultraviolet, near ultraviolet excitation after grinding evenly.
3. a preparation method for a kind of orange red antimonate luminescent materials as claimed in claim 2, is characterized in that: the precalcining temperature of step (2) is 350 ~ 650 DEG C, and the precalcining time is 3 ~ 12 hours.
4. a preparation method for a kind of orange red antimonate luminescent materials as claimed in claim 2, is characterized in that: the calcining temperature of step (3) is 750 ~ 1000 DEG C, and calcination time is 2 ~ 9 hours.
5. a preparation method for a kind of orange red antimonate luminescent materials as claimed in claim 2, is characterized in that: described calcium ions Ca 2+compound be one in calcium carbonate, calcium chloride, nitrocalcite, calcium hydroxide, calcium oxide; Described contains europium ion Eu 3+compound be one in europium sesquioxide, europium nitrate, Europium trichloride; Described contains antimony ion Sb 3+compound be one in antimonous oxide, antimony chloride or nitric acid antimony.
6. a preparation method for a kind of orange red antimonate luminescent materials as claimed in claim 1, adopts chemical synthesis, it is characterized in that comprising the steps:
(1) by chemical formula Ca 5-5xeu 5xsb 5o 17in the stoichiometric ratio of each element, wherein 0.001≤x≤0.15, takes respectively containing calcium ion Ca 2+compound, containing europium ion Eu 3+compound, containing antimony ion Sb 3+compound, they are used dust technology and deionized water dissolving respectively, then add complexing agent citric acid or oxalic acid respectively by 0.5 ~ 2.0wt% of each reactant quality, obtain the mixing solutions of each raw material;
(2) each mixing solutions that step (1) obtains slowly is mixed, then under the temperature condition of 50 ~ 80 DEG C stir 1 ~ 2 hour, leave standstill, dry after obtain bulk presoma;
(3) presoma that step (2) obtains is placed in retort furnace to calcine, calcining temperature is 500 ~ 950 DEG C, calcination time is 2 ~ 10 hours, naturally cools to room temperature, obtains a kind of stibnate luminescent material can launching orange red light under ultraviolet, near ultraviolet excitation after grinding evenly.
7. the preparation method of a kind of orange red antimonate luminescent materials according to claim 6, is characterized in that: the calcining temperature of step (3) is 600 ~ 900 DEG C, and calcination time is 3 ~ 9 hours.
8. the preparation method of a kind of orange red antimonate luminescent materials according to claim 6, is characterized in that: described calcium ions Ca 2+compound be one in calcium carbonate, calcium chloride, nitrocalcite, calcium hydroxide, calcium oxide; Described contains europium ion Eu 3+compound be one in europium sesquioxide, europium nitrate, Europium trichloride; Described contains antimony ion Sb 3+compound be one in antimonous oxide, antimony chloride or nitric acid antimony.
9. an application for orange red antimonate luminescent materials, is characterized in that: be applied to the adjustment with photoluminescence colourity in various luminouslighting material.
CN201510979018.5A 2015-12-23 2015-12-23 A kind of preparation method and application of orange red antimonate luminescent materials Active CN105419798B (en)

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CN109825296A (en) * 2019-03-05 2019-05-31 常州工程职业技术学院 A kind of europium ion Eu3+Fluorine antimonate orange red fluorescent powder of activation and preparation method thereof
CN113583672A (en) * 2021-07-21 2021-11-02 厦门理工学院 Eu3+Doped composite antimonate red fluorescent powder and preparation method and application thereof

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CN113583672B (en) * 2021-07-21 2023-04-14 厦门理工学院 Eu 3+ Doped composite antimonate red fluorescent powder and preparation method and application thereof

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