CN104910908A - Red fluorescent material for white light LED and preparation method thereof - Google Patents
Red fluorescent material for white light LED and preparation method thereof Download PDFInfo
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- CN104910908A CN104910908A CN201510234227.7A CN201510234227A CN104910908A CN 104910908 A CN104910908 A CN 104910908A CN 201510234227 A CN201510234227 A CN 201510234227A CN 104910908 A CN104910908 A CN 104910908A
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- 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
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Abstract
The invention discloses a red fluorescent material for a white light LED, which has a chemical formula of Ba3-3xEu3xMgSb2O9Wherein x is Eu3+The doping mole percentage is that x is more than or equal to 0.0001 and less than or equal to 0.15. The luminescent material of the invention is prepared by adopting a high-temperature solid phase method or a chemical synthesis method and taking novel antimonate as a matrix material, and the prepared red fluorescent materialThe powder can be excited by light with the wavelength of 250-470 nanometers and emits red light with the main wavelength of 616 nanometers. The raw materials used in the invention are cheap and easily available, the preparation process is simple and flexible, the requirement on equipment is not high, the production cost is greatly reduced, and the method is suitable for large-scale production, energy-saving and environment-friendly; the prepared fluorescent powder has high purity, good crystallinity, stable performance, excellent luminous performance and stronger visible light transmission, and has wide application prospect in the field of LED illumination.
Description
Technical field
The present invention relates to a kind of luminescent material and preparation method thereof, particularly a kind of white light LEDs red fluorescence material and preparation method thereof, belongs to luminescent material technical field.
Background technology
Since 21 century, energy saving standard is the topic that Sustainable Socioeconomic Development is talked about always.Compared to traditional electricity-saving lamp, white light LEDs by feat of energy-efficient, stable performance, long service life, to advantages such as environment do not pollute, be described as the green light source of 21st century, becomes one of focus of people's research in lighting field.
The white light LEDs generally used in the market is mainly with the fluorescent material of blue-light LED chip collocation YAG:Ce, to launch by exciting YAG:Ce that gold-tinted and blue light realize, but because it lacks red color light component, cause its colour rendering index lower, color reducibility is poor, and colour temperature is higher.In numerous lamp red fluorescence powders, real practicality and few, the red fluorescence powder that effectively can be excited by near-ultraviolet light is little, and particularly after its physical chemistry comprehensive, luminous efficiency, thermostability, the red fluorescence powder that can be used near ultraviolet white light LEDs just lacks more; Meanwhile, existing commercial fluorescent material is matrix mainly with sulfide, halogenide, and the preparation method of these materials is much more complicated and not environmentally, the high efficiency red fluorescent material therefore developing good combination property becomes the focus of research both at home and abroad at present.
Summary of the invention
For the deficiency that above-mentioned prior art exists, the object of this invention is to provide that a kind of preparation manipulation simple and flexible, luminous efficiency are high, good stability and environment amenable white light LEDs red fluorescence material and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is: provide a kind of white light LEDs red fluorescence material, and chemical formula is Ba
3-3xeu
3xmgSb
2o
9, wherein x is Eu
3+the molecular fraction of doping, 0.0001≤x≤0.15.
The present invention provides the preparation method of above-mentioned white light LEDs red fluorescence material simultaneously, adopts high temperature solid-state method preparation, comprises the steps:
(1) with containing barium ion Ba
2+compound, containing europium ion Eu
3+compound, containing magnesium ion Mg
2+compound, containing antimony ion Sb
5+compound be raw material, by chemical formula Ba
3-3xeu
3xmgSb
2o
9the stoichiometric ratio of middle corresponding element takes each raw material, and wherein 0.0001≤x≤0.15 is ground and mixes, obtaining mixture;
(2) mixture is placed in retort furnace, in air atmosphere precalcining, precalcining temperature is 500 ~ 900 DEG C, 2 ~ 16 hours precalcining time;
(3) mixture that step (2) obtains is naturally cooled to room temperature, grind and mix, again be placed in retort furnace, calcine in air atmosphere, calcining temperature 900 ~ 1500 DEG C, calcination time 1 ~ 12 hour, naturally cools to room temperature, obtains luminescent material after grinding evenly.
Preferably, in the step (2) of high temperature solid-state method of the present invention, precalcining temperature is 550 ~ 850 DEG C, and the precalcining time is 3 ~ 12 hours.
Preferably, step (3) calcining temperature of high temperature solid-state method of the present invention is 950 ~ 1400 DEG C, and calcination time is 2 ~ 9 hours.
In the technical scheme of high temperature solid-state method of the present invention, containing barium ion Ba
2+compound be one in barium oxide, bariumchloride, nitrate of baryta, barium carbonate, hydrated barta; Containing europium ion Eu
3+compound be one in europium sesquioxide, europium nitrate; Containing magnesium ion Mg
2+compound be one in magnesium oxide, magnesium chloride, magnesium nitrate, magnesium basic carbonate; Containing antimony ion Sb
5+compound be one in antimony peroxide, antimony chloride or antimony trisulfate.
The present invention also provides above-mentioned white light LEDs red fluorescence material another kind of preparation method simultaneously, adopts chemical synthesis preparation, comprises the steps:
(1) with containing barium ion Ba
2+compound, containing europium ion Eu
3+compound, containing magnesium ion Mg
2+compound, containing antimony ion Sb
5+compound be raw material, by chemical formula Ba
3-3xeu
3xmgSb
2o
9the stoichiometric ratio of middle corresponding element takes each raw material, and wherein x is Eu
3+the molecular fraction of doping, 0.0001≤x≤0.15, use dust technology and each raw material of deionized water dissolving respectively, then add complexing agent respectively by 0.5 ~ 2.0wt% of each raw materials quality, stir, described complexing agent is citric acid or oxalic acid;
(2) each solution 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 ~ 1000 DEG C, and calcination time 2 ~ 10 hours, naturally cools to room temperature, obtains luminescent material after grinding evenly.
Preferably, the calcining temperature of the step (3) of chemical synthesis of the present invention is 600 ~ 900 DEG C, and calcination time is 3 ~ 9 hours.
In the technical scheme of chemical synthesis of the present invention, containing barium ion Ba
2+compound be one in barium oxide, bariumchloride, nitrate of baryta, barium carbonate, hydrated barta; Containing europium ion Eu
3+compound be one in europium sesquioxide, europium nitrate; Containing magnesium ion Mg
2+compound be one in magnesium oxide, magnesium chloride, magnesium nitrate, magnesium basic carbonate; Containing antimony ion Sb
5+compound be one in antimony peroxide, antimony chloride or antimony trisulfate.
Compared with prior art, tool of the present invention has the following advantages:
1, red fluorescence material provided by the invention is using the stibnate of stable chemical nature as substrate material, it has good charge-transfer absorption band in near-ultraviolet light district, after exciting by the transmission ofenergy of absorption to the rare earth ion be entrained in barium magnesium stibnate, its antimony acid radical anion can meet the requirement of fluorescent material to light transmission fully.Material purity of the present invention is high, can by the optical excitation of wavelength in 250 ~ 470 nanometer range, and launch the ruddiness of main peak at 616 nm, colourity is pure, stable performance, can be applied in novel white-light LED.
2, red fluorescence material preparation process simple and flexible provided by the invention; favorable repeatability; and in whole process, do not need reducing atmosphere to protect; because this reducing energy consumption; and less demanding for equipment, cheaper starting materials is easy to get, and also greatly reduces production cost; relative to the fluorescent material such as sulfide, halide based, more environmental protection.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction pattern of the sample prepared by the embodiment of the present invention 1 technical scheme;
Fig. 2 is the scanning electron microscope diagram spectrum of the sample prepared by the embodiment of the present invention 1 technical scheme;
Fig. 3 is the exciting light spectrogram that the sample prepared by the embodiment of the present invention 1 technical scheme obtains under the light detection of 616 nanometers;
Fig. 4 is the luminescent spectrum figure of sample under the optical excitation of 395 nanometers prepared by the embodiment of the present invention 1 technical scheme;
Fig. 5 is the sample prepared by the embodiment of the present invention 1 technical scheme is 395 nanometers in excitation wavelength, and monitoring wavelength is the decay of luminescence curve of 616 nanometers;
Fig. 6 is the X-ray powder diffraction pattern of the sample prepared by the embodiment of the present invention 5 technical scheme;
Fig. 7 is the scanning electron microscope diagram spectrum of the sample prepared by the embodiment of the present invention 5 technical scheme;
Fig. 8 is the exciting light spectrogram that the sample prepared by the embodiment of the present invention 5 technical scheme obtains under the light detection of 615 nanometers;
Fig. 9 is the luminescent spectrum figure of sample under the optical excitation of 395 nanometers prepared by the embodiment of the present invention 5 technical scheme;
Figure 10 is the sample prepared by the embodiment of the present invention 5 technical scheme is 395 nanometers in excitation wavelength, and monitoring wavelength is the decay of luminescence curve of 615 nanometers.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Embodiment 1:
Preparation Ba
2.7eu
0.3mgSb
2o
9, according to chemical formula Ba
2.7eu
0.3mgSb
2o
9in the stoichiometric ratio of each element, take barium carbonate BaCO respectively
3: 1.3321 grams, europium sesquioxide Eu
2o
3: 0.1319 gram, magnesium oxide MgO:0.1008 gram, antimony peroxide Sb
2o
5: 0.8088 gram, to grind in agate mortar and after mixing, select air atmosphere precalcining 3 hours at 850 DEG C in retort furnace, naturally cool to room temperature, take out sample; Abundant mixed grinding is even, is again placed in retort furnace, and among air atmosphere, 1400 DEG C of calcinings 2 hours, naturally cool to room temperature, after taking out, fully namely grinding evenly obtains powdered luminescent materials.
See accompanying drawing 1, it is the X-ray powder diffraction pattern that the present embodiment technical scheme prepares sample, and test result shows, occur without other assorted peak in figure, contrast with the card PDF#45-0898 of standard, the position of diffraction peak is all consistent with standard card with relative intensity, and prepared material principal phase is Ba
3mgSb
2o
9, illustrate that the sample obtained by this example is pure thing phase, crystallinity is good.
See accompanying drawing 2, it is composed by the scanning electron microscope diagram of sample prepared by the present embodiment technical scheme, and as can be seen from the figure, gained sample good crystallinity, Granular composite is even, and its median size is 7.60 microns.
See accompanying drawing 3, it is the exciting light spectrogram of sample under the light detection of 616 nanometers prepared by the present embodiment technical scheme, and as seen from the figure, this material well can be excited by the light of wavelength in 250 ~ 470 nanometer range.
See accompanying drawing 4, it is the luminescent spectrum figure that the sample prepared by the present embodiment technical scheme obtains under the optical excitation of 395 nanometers, and as seen from the figure, this material can launch the ruddiness of predominant wavelength at 616 nm.
See accompanying drawing 5, it is the sample prepared by the present embodiment technical scheme is 395 nanometers in excitation wavelength, and monitoring wavelength is the decay of luminescence curve of 616 nanometers, and can be calculated fall time is 1.37 milliseconds.
Embodiment 2:
Preparation Ba
2.64eu
0.36mgSb
2o
9, according to chemical formula Ba
2.64eu
0.36mgSb
2o
9in the stoichiometric ratio of each element, take nitrate of baryta Ba (NO respectively
3)
2: 1.7248 grams, europium sesquioxide Eu
2o
3: 0.1584 gram, magnesium basic carbonate 4MgCO
3mg (OH)
25H
2o:0.2429 gram, antimony peroxide Sb
2o
5: 0.8088 gram, to grind in agate mortar and after mixing, select air atmosphere precalcining 2 hours at 900 DEG C in retort furnace, naturally cool to room temperature, take out sample; Abundant mixed grinding is even, is again placed in retort furnace, and among air atmosphere, 1500 DEG C of calcinings 1 hour, naturally cool to room temperature, after taking out, fully namely grinding evenly obtains powdered luminescent materials.
Sample prepared by the present embodiment, its primary structure pattern, excitation spectrum, emmission spectrum and decay of luminescence curve are similar to embodiment 1.
Embodiment 3:
Preparation Ba
2.55eu
0.45mgSb
2o
9, according to chemical formula Ba
2.55eu
0.45mgSb
2o
9in the stoichiometric ratio of each element, take barium oxide BaO:0.9775 gram respectively, europium sesquioxide Eu
2o
3: 0.1979 gram, magnesium oxide MgO:0.1008 gram, antimony peroxide Sb
2o
5: 0.8088 gram, to grind in agate mortar and after mixing, select air atmosphere precalcining 16 hours at 500 DEG C in retort furnace, naturally cool to room temperature, take out sample; Abundant mixed grinding is even, is again placed in retort furnace, and among air atmosphere, calcine 12 hours, naturally cool to room temperature at 900 DEG C, after taking out, fully namely grinding evenly obtains powdered luminescent materials.
Sample prepared by the present embodiment, its primary structure pattern, excitation spectrum, emmission spectrum and decay of luminescence curve are similar to embodiment 1.
Embodiment 4:
Preparation Ba
2.76eu
0.24mgSb
2o
9, according to chemical formula Ba
2.76eu
0.24mgSb
2o
9in the stoichiometric ratio of each element, take hydrated barta Ba (OH) respectively
2: 1.1823 grams, europium sesquioxide Eu
2o
3: 0.1055 gram, magnesium basic carbonate 4MgCO
3mg (OH)
25H
2o:0.2429 gram, antimony peroxide Sb
2o
5: 0.8088 gram, to grind in agate mortar and after mixing, select air atmosphere precalcining 12 hours at 550 DEG C in retort furnace, naturally cool to room temperature, take out sample; Abundant mixed grinding is even, is again placed in retort furnace, and among air atmosphere, 950 DEG C of calcinings 9 hours, naturally cool to room temperature, after taking out, fully namely grinding evenly obtains powdered luminescent materials.
Sample prepared by the present embodiment, its primary structure pattern, excitation spectrum, emmission spectrum and decay of luminescence curve are similar to embodiment 1.
Embodiment 5:
Preparation Ba
2.85eu
0.15mgSb
2o
9, according to chemical formula Ba
2.85eu
0.15mgSb
2o
9in the stoichiometric ratio of each element, take bariumchloride BaCl respectively
2: 1.4836 grams, europium nitrate Eu (NO
3)
36H
2o:0.1267 gram, magnesium nitrate Mg (NO
3)
26H
2o:0.6410 gram, antimony chloride SbCl
3: 1.1416 grams, then the citric acid taking above each raw materials quality 2.0wt% respectively.Use appropriate deionized water and dilute nitric acid dissolution above-mentioned raw materials respectively, and then add the citric acid taken respectively and carry out complexing, stir; By dissolution homogeneity good for above-mentioned complexing mix, be heated to 80 DEG C and stir 1 hour, leave standstill, dry after obtain bulk presoma; Presoma is placed in retort furnace calcine, calcining temperature is 900 DEG C, and calcination time 3 hours, naturally cools to room temperature, and after taking out, namely grinding evenly obtains powdered luminescent materials.
See accompanying drawing 6, it is the X-ray powder diffraction pattern that the present embodiment technical scheme prepares sample, and test result shows, occur without other assorted peak in figure, contrast with the card PDF#45-0898 of standard, the position of diffraction peak is all consistent with standard card with relative intensity, and prepared material principal phase is Ba
3mgSb
2o
9, illustrate that the sample obtained by this example is pure thing phase, crystallinity is good.
See accompanying drawing 7, it is composed by the scanning electron microscope diagram of sample prepared by the present embodiment technical scheme, and as can be seen from the figure, gained sample particle is uniformly dispersed, and its median size is 1.45 microns.
See accompanying drawing 8, it is the exciting light spectrogram of sample under the light detection of 615 nanometers prepared by the present embodiment technical scheme, and find out by figure, this material well can be excited by the light of wavelength in 250 ~ 470 nanometer range.
See accompanying drawing 9, it is the luminescent spectrum figure that the sample prepared by the present embodiment technical scheme obtains under the optical excitation of 395 nanometers, and by Tu Ke get, this material can launch the ruddiness of predominant wavelength at 615 nm.
See accompanying drawing 10, it is the sample prepared by the present embodiment technical scheme is 395 nanometers in excitation wavelength, and monitoring wavelength is the decay of luminescence curve of 615 nanometers, and can be calculated fall time is 1.13 milliseconds.
Embodiment 6:
Preparation Ba
2.94eu
0.06mgSb
2o
9, according to chemical formula Ba
2.94eu
0.06mgSb
2o
9in the stoichiometric ratio of each element, take hydrated barta Ba (OH) respectively
2: 1.2594 grams, europium nitrate Eu (NO
3)
36H
2o:0.0506 gram, magnesium chloride Mg Cl
26H
2o:0.5080 gram, antimony trisulfate Sb
2(SO
4)
3: 1.3292 grams, then the citric acid taking above each raw materials quality 0.5wt% respectively.Use appropriate deionized water and dilute nitric acid dissolution above-mentioned raw materials respectively, and then add the citric acid taken respectively and carry out complexing, stir; By dissolution homogeneity good for above-mentioned complexing mix, be heated to 50 DEG C and stir 2 hours, leave standstill, dry after obtain bulk presoma; Presoma is placed in retort furnace calcine, calcining temperature is 1000 DEG C, and calcination time 2 hours, naturally cools to room temperature, and after taking out, namely grinding evenly obtains powdered luminescent materials.
Sample prepared by the present embodiment, its primary structure pattern, excitation spectrum, emmission spectrum and extinction curve are similar to embodiment 5.
Embodiment 7:
Preparation Ba
2.97eu
0.03mgSb
2o
9, according to chemical formula Ba
2.97eu
0.03mgSb
2o
9in the stoichiometric ratio of each element, take nitrate of baryta Ba (NO respectively
3)
2: 1.9404 grams, europium nitrate Eu (NO
3)
36H
2o:0.0253 gram, magnesium nitrate Mg (NO
3)
26H
2o:0.6410 gram, antimony trisulfate Sb
2(SO
4)
3: 1.3292 grams, then the oxalic acid taking above each raw materials quality 2.0wt% respectively.Use appropriate deionized water and dilute nitric acid dissolution above-mentioned raw materials respectively, and then add the oxalic acid taken respectively and carry out complexing, stir; By dissolution homogeneity good for above-mentioned complexing mix, be heated to 60 DEG C and stir 1.5 hours, leave standstill, dry after obtain bulk presoma; Presoma is placed in retort furnace calcine, calcining temperature is 500 DEG C, and calcination time 10 hours, naturally cools to room temperature, and after taking out, namely grinding evenly obtains powdered luminescent materials.
Sample prepared by the present embodiment, its primary structure pattern, excitation spectrum, emmission spectrum and extinction curve are similar to embodiment 5.
Embodiment 8:
Preparation Ba
2.997eu
0.003mgSb
2o
9, according to chemical formula Ba
2.997eu
0.003mgSb
2o
9in the stoichiometric ratio of each element, take nitrate of baryta Ba (NO respectively
3)
2: 1.9580 grams, europium nitrate Eu (NO
3)
36H
2o:0.0025 gram, magnesium chloride Mg Cl
26H
2o:0.5080 gram, antimony peroxide Sb
2o
5: 0.8088 gram, then the oxalic acid taking above each raw materials quality 0.5wt% respectively.Use appropriate deionized water and dilute nitric acid dissolution above-mentioned raw materials respectively, and then add the oxalic acid taken respectively and carry out complexing, stir; By dissolution homogeneity good for above-mentioned complexing mix, be heated to 60 DEG C and stir 2 hours, leave standstill, dry after obtain bulk presoma; Presoma is placed in retort furnace calcine, calcining temperature is 650 DEG C, and calcination time 8 hours, naturally cools to room temperature, and after taking out, namely grinding evenly obtains powdered luminescent materials.
Sample prepared by the present embodiment, its primary structure pattern, excitation spectrum, emmission spectrum and extinction curve are similar to embodiment 5.
Embodiment 9:
Preparation Ba
2.9997eu
0.0003mgSb
2o
9, according to chemical formula Ba
2.9997eu
0.0003mgSb
2o
9in the stoichiometric ratio of each element, take bariumchloride BaCl respectively
2: 1.5616 grams, europium nitrate Eu (NO
3)
36H
2o:0.0003, magnesium nitrate Mg (NO
3)
26H
2o:0.6410 gram, antimony peroxide Sb
2o
5: 0.8088 gram, then the citric acid taking above each raw materials quality 2.0wt% respectively.Use appropriate deionized water and dilute nitric acid dissolution above-mentioned raw materials respectively, and then add the citric acid taken respectively and carry out complexing, stir; By dissolution homogeneity good for above-mentioned complexing mix, be heated to 80 DEG C and stir 2 hours, leave standstill, dry after obtain bulk presoma; Presoma is placed in retort furnace calcine, calcining temperature is 600 DEG C, and calcination time 9 hours, naturally cools to room temperature, and after taking out, namely grinding evenly obtains powdered luminescent materials.
Sample prepared by the present embodiment, its primary structure pattern, excitation spectrum, emmission spectrum and extinction curve are similar to embodiment 5.
Claims (8)
1. a white light LEDs red fluorescence material, is characterized in that: chemical formula is Ba
3-3xeu
3xmgSb
2o
9, wherein x is Eu
3+the molecular fraction of doping, 0.0001≤x≤0.15.
2. a preparation method for white light LEDs red fluorescence material as claimed in claim 1, is characterized in that, adopts high temperature solid-state method, comprises the steps:
(1) with containing barium ion Ba
2+compound, containing europium ion Eu
3+compound, containing magnesium ion Mg
2+compound, containing antimony ion Sb
5+compound be raw material, by chemical formula Ba
3-3xeu
3xmgSb
2o
9the stoichiometric ratio of middle corresponding element takes each raw material, and wherein 0.0001≤x≤0.15 is ground and mixes, obtaining mixture;
(2) mixture is placed in retort furnace, in air atmosphere precalcining, precalcining temperature is 500 ~ 900 DEG C, 2 ~ 16 hours precalcining time;
(3) mixture that step (2) obtains is naturally cooled to room temperature, grind and mix, again be placed in retort furnace, calcine in air atmosphere, calcining temperature 900 ~ 1500 DEG C, calcination time 1 ~ 12 hour, naturally cools to room temperature, obtains luminescent material after grinding evenly.
3. the preparation method of white light LEDs red fluorescence material according to claim 2, is characterized in that: the precalcining temperature of step (2) is 550 ~ 850 DEG C, and the precalcining time is 3 ~ 12 hours.
4. the preparation method of white light LEDs red fluorescence material according to claim 2, is characterized in that: the calcining temperature of step (3) is 950 ~ 1400 DEG C, and calcination time is 2 ~ 9 hours.
5. the preparation method of white light LEDs red fluorescence material according to claim 2, is characterized in that: described contains barium ion Ba
2+compound be one in barium oxide, bariumchloride, nitrate of baryta, barium carbonate, hydrated barta; Containing europium ion Eu
3+compound be one in europium sesquioxide, europium nitrate; Containing magnesium ion Mg
2+compound be one in magnesium oxide, magnesium chloride, magnesium nitrate, magnesium basic carbonate; Containing antimony ion Sb
5+compound be one in antimony peroxide, antimony chloride or antimony trisulfate.
6. a preparation method for white light LEDs red fluorescence material as claimed in claim 1, is characterized in that, adopts chemical synthesis, comprises the steps:
(1) with containing barium ion Ba
2+compound, containing europium ion Eu
3+compound, containing magnesium ion Mg
2+compound, containing antimony ion Sb
5+compound be raw material, by chemical formula Ba
3-3xeu
3xmgSb
2o
9the stoichiometric ratio of middle corresponding element takes each raw material, and wherein x is Eu
3+the molecular fraction of doping, 0.0001≤x≤0.15, use dust technology and each raw material of deionized water dissolving respectively, then add complexing agent respectively by 0.5 ~ 2.0wt% of each raw materials quality, stir, described complexing agent is citric acid or oxalic acid;
(2) each solution 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 ~ 1000 DEG C, and calcination time 2 ~ 10 hours, naturally cools to room temperature, obtains luminescent material after grinding evenly.
7. the preparation method of white light LEDs red fluorescence material 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 white light LEDs red fluorescence material according to claim 6, is characterized in that: described contains barium ion Ba
2+compound be one in barium oxide, bariumchloride, nitrate of baryta, barium carbonate, hydrated barta; Containing europium ion Eu
3+compound be one in europium sesquioxide, europium nitrate; Containing magnesium ion Mg
2+compound be one in magnesium oxide, magnesium chloride, magnesium nitrate, magnesium basic carbonate; Containing antimony ion Sb
5+compound be one in antimony peroxide, antimony chloride or antimony trisulfate.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105419799A (en) * | 2015-12-23 | 2016-03-23 | 江苏师范大学 | Preparation method and application of material for converting near ultraviolet light to emit red fluorescence |
| CN105838368A (en) * | 2016-05-26 | 2016-08-10 | 江苏爱福特科技开发有限公司 | Fluorescent material for white light LED and preparation method of fluorescent material |
| CN106047345A (en) * | 2016-05-26 | 2016-10-26 | 江苏爱福特科技开发有限公司 | Red fluorescent material and preparation method thereof |
| 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006068359A1 (en) * | 2004-12-22 | 2006-06-29 | Seoul Semiconductor Co., Ltd. | Light emitting device |
| US20070035813A1 (en) * | 2002-12-20 | 2007-02-15 | Gundula Roth | Phosphor and optical device using same |
| CN103627392A (en) * | 2013-11-19 | 2014-03-12 | 苏州大学 | Antimonate-based red phosphor powder and preparation method and application thereof |
| CN103865532A (en) * | 2014-03-31 | 2014-06-18 | 长安大学 | Double-ion-doped antimonate luminescent material and preparation method thereof |
| CN104277842A (en) * | 2013-07-12 | 2015-01-14 | 海洋王照明科技股份有限公司 | Europium-terbium-codoped titanium antimonate light-emitting film, and preparation method and application of europium-terbium-codoped titanium antimonate light-emitting film |
-
2015
- 2015-05-08 CN CN201510234227.7A patent/CN104910908B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070035813A1 (en) * | 2002-12-20 | 2007-02-15 | Gundula Roth | Phosphor and optical device using same |
| WO2006068359A1 (en) * | 2004-12-22 | 2006-06-29 | Seoul Semiconductor Co., Ltd. | Light emitting device |
| CN104277842A (en) * | 2013-07-12 | 2015-01-14 | 海洋王照明科技股份有限公司 | Europium-terbium-codoped titanium antimonate light-emitting film, and preparation method and application of europium-terbium-codoped titanium antimonate light-emitting film |
| CN103627392A (en) * | 2013-11-19 | 2014-03-12 | 苏州大学 | Antimonate-based red phosphor powder and preparation method and application thereof |
| CN103865532A (en) * | 2014-03-31 | 2014-06-18 | 长安大学 | Double-ion-doped antimonate luminescent material and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105419799A (en) * | 2015-12-23 | 2016-03-23 | 江苏师范大学 | Preparation method and application of material for converting near ultraviolet light to emit red fluorescence |
| CN105838368A (en) * | 2016-05-26 | 2016-08-10 | 江苏爱福特科技开发有限公司 | Fluorescent material for white light LED and preparation method of fluorescent material |
| CN106047345A (en) * | 2016-05-26 | 2016-10-26 | 江苏爱福特科技开发有限公司 | Red fluorescent material and preparation method thereof |
| 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 |
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