CN103146386A - Europium doped lanthanide silicon oxynitride and preparation method thereof - Google Patents
Europium doped lanthanide silicon oxynitride and preparation method thereof Download PDFInfo
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- CN103146386A CN103146386A CN2013100826318A CN201310082631A CN103146386A CN 103146386 A CN103146386 A CN 103146386A CN 2013100826318 A CN2013100826318 A CN 2013100826318A CN 201310082631 A CN201310082631 A CN 201310082631A CN 103146386 A CN103146386 A CN 103146386A
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Abstract
The invention discloses a europium doped lanthanide silicon oxynitride, of which the chemical general formula is La5-5xEu5xSi3O12N, wherein x is more than 0 and less than 0.25. The preparation method comprises the steps of: (a) weighing raw materials: lanthanum trioxide, silicon dioxide, silicon nitride and europium oxide, according to the molar ratio of the chemical formula La5-5xEu5xSi3O12N (x is more than 0 and less than 0.25); (b) ball-milling the raw materials and tabletting; (c) putting tablets into a high temperature furnace, under the nitrogen hydrogen atmosphere, raising the furnace temperature to 1000-1250 DEG C, and sintering for 3-10 hours; (d) turning off a hydrogen source, under the environment of charging nitrogen gas, keeping the high temperature furnace at a pressure of 0.5-1MPa, raising the furnace temperature to 1450-1550 DEG C, and continuously sintering the tablets for 3-10 hours; and (e) ventilating to release the pressure in the furnace to be an ordinary pressure, cooling down the high temperature furnace to room temperature by circulating under the nitrogen-hydrogen mixed atmosphere, taking out the sample tablets, and grinding, thus obtaining a fluorescent material. The fluorescent material prepared by the preparation method is stable in physicochemical property, convenient to control luminescence property, simple in preparation method, and free from environmental pollution, and is applicable to industrialized mass production.
Description
Technical field
The present invention relates to fluorescent material that contains in rare earth metal and preparation method thereof, specifically a kind of europium doping group of the lanthanides silica nitrogen compound and preparation method thereof.
Background technology
The advantages such as white light LEDs is little due to volume, energy-saving and environmental protection, long lifetime cause people's extensive concern, are called as lighting source of new generation.At present, White-light LED illumination is mainly realized by the light transformation way, namely excites yellow fluorescent powder by blue chip, and blue, yellow light mix obtains white light, perhaps excite three kinds of fluorescent material of red, green, blue by purple light (or UV-light), red, green-blue light is mixed into white light.For this reason, the technician has developed in continuous research and multiplely can present the fluorescent material of versicolor visible light under rayed.
Nitride fluorescent material is because it has nontoxic, not deliquescence and thermostability advantages of higher, becomes one of focus of luminescent material research field in recent years.Bond energy of covalent bond due to the nitrogen ion in nitride is higher, so its Stability Analysis of Structures, resistance of oxidation are strong, erosion resistance, are the good matrix of rare earth doping fluorescent material.The La-Si-O-N compound is a kind of in the fluorescent material nitride substrate, its abundant species, and structural formula is various.At present, more existing europiums are entrained in and make the luminescent properties application of fluorescent material preferably in nitride on the market.Disclose a kind of nitric oxide fluorescent powder of mixing europium as CN101434839A, the chemical general formula of this fluorescent material is { M
(1-x)Eu
x}
aSi
bO
cN
d, wherein, M is Ba, Sr or Ca, 0＜x＜1,1.8＜a＜2.2,4.5＜b＜5.5,0＜c＜8,0＜d≤8,0＜c+d≤8, and this material is the fluorescent chemicals that luminous efficiency is good, can glow; Separately there is CN102260502A to disclose a kind of (Ca, Mg) Si
2ON:Eu
2+Fluorescent material and preparation method thereof, be with raw material mix, dry, filter, calcining, pulverize, make (Ca, Mg) Si of the green glow that can turn to be yellow
2ON:Eu
2+Fluorescent material; And in existing research, also do not find Eu
2+Be entrained in La-Si-O-N matrix, preparation can be launched the relevant report of the fluorescent chemicals of blue green light.
Summary of the invention
Purpose of the present invention just is to provide a kind of europium doping group of the lanthanides silica nitrogen compound and preparation method thereof, with develop a kind of Spectral matching good, with spectrum width, can launch the novel fluorescent material of blue green light.
The objective of the invention is to be achieved through the following technical solutions:
A kind of europium doping group of the lanthanides silica nitrogen compound, its chemical general formula is: La
5-5xEu
5xSi
3O
12N, wherein, 0＜x＜0.25.
Preferred 0＜x＜0.1 in chemical general formula described in the present invention.
A kind of preparation method of europium doping group of the lanthanides silica nitrogen compound, it comprises the following steps preparation:
(a) according to chemical formula La
5-5xEu
5xSi
3O
12N, wherein mole proportioning raw materials weighing of 0＜x＜0.25: lanthanum sesquioxide, silicon-dioxide, silicon nitride, europiumsesquioxide;
(b) raw material is carried out ball milling, the powder after ball milling carries out compressing tablet;
(c) compressing tablet is placed in High Temperature Furnaces Heating Apparatus, is filled with nitrogen, hydrogen mixing source of the gas in stove, furnace temperature is risen to 1000～1250 ℃, sintering 3～10 hours;
(d) turn off hydrogen source gas, under the environment of the source of the gas that is filled with nitrogen, the air pressure of High Temperature Furnaces Heating Apparatus maintains under 0.5～1MPa, and furnace temperature rises to 1450～1550 ℃, and compressing tablet was continued sintering 3～10 hours;
(e) ventilation makes the pressure in High Temperature Furnaces Heating Apparatus reduce to normal pressure, under the circulation in nitrogen and hydrogen mixture source, makes High Temperature Furnaces Heating Apparatus naturally be down to room temperature, takes out compressing tablet, grinds, and namely gets fluorescent material.
Preferred 0＜x＜0.1 in step of the present invention (a), its x is in this scope, and the luminescent properties of the fluorescent material of preparation is relatively stronger.
The described Ball-milling Time of step of the present invention (b) is 1～2 hour, and its ball milling can make reaction raw materials fully mix contact, and Ball-milling Time is too short, and the reaction raw materials mixedness is inadequate; Ball-milling Time is oversize, and reaction raw materials is easy to reunite, and also is unfavorable for abundant reaction.
During step of the present invention (b) compressing tablet, pressure is 13～18MPa; Pressure is too little, is unfavorable for reaction; Pressure is too large, easily destroys lattice, and the sample luminous intensity after sintering can be died down.
Preferred 3 hours of the described sintering time of step of the present invention (c) can make reaction comparatively abundant, and preparation efficiency is higher.
Preferred 3 hours of the described sintering time of step of the present invention (d) can make reaction comparatively abundant, and preparation efficiency is higher.
The air pressure of the described High Temperature Furnaces Heating Apparatus of step of the present invention (d) has the environment of pressure at 0.5MPa, and the raw material reaction degree is better, and when air pressure was low, level of response was bad or need the longer reaction times; Limited by technical qualification, when satisfying reaction requirement, institute adds air pressure and is difficult for too high.
Europium doping group of the lanthanides silica nitrogen compound provided by the invention has following characteristics:
(1) fluorescent material grating spectrum of the present invention and La
5Si
3O
12N standard card coupling is fine, does not have other dephasigns to exist, and only comprises a kind of urstoff;
(2) excitation spectrum of fluorescent material of the present invention presents the wideband spectrum structure, excites approximately 340nm of peak position; This fluorescent material can effectively be excited in the 250-450nm wavelength region;
(3) emmission spectrum of fluorescent material of the present invention is unimodal wideband spectrum structure, and the emmission spectrum frequency band approximately is in 450～650nm scope, and the emission peak position is 510nm approximately.
In the present invention, europium belongs to the element in group of the lanthanides, Eu
2+Be the low price rare earth ion that belongs to abnormal valence state, mix Eu
2+Solid chemical compound all is widely used at aspects such as low price rare-earth luminescent material, long after glow luminous material, photostimulated phosphors.But Eu
2+Stronger reductibility is arranged, less stable, Eu in oxide system
2+Doped and substituted make lattice that serious distortion occur, and valence state can not stable existence in parent lattice, easily change Eu into
3+Therefore, in the factor that affects the rare earth valence stability, the selection of substrate material and the method for preparing lattice are vital for the stable ion of rare earth Eu at a low price.The present invention under high-temperature and high-pressure conditions, adopts the La-Si-O-N compound as matrix by specific preparation method, has reached first Eu
2+The purpose of stable existence in La (group of the lanthanides)-Si-O-N matrix has successfully been developed the La that can launch blue green light
5Si
3O
12N:Eu
2+Fluorescent chemicals.
The optical detection of fluorescent chemicals provided by the invention shows to have strong emission peak at 450～650nm wave band, and the emission peak position is 510nm approximately, the emission blue green light; Have strong excitation peak in 250～450nm wavelength region, excite approximately 340nm of peak position, can effectively be excited by purple light or ultraviolet leds chip.
Raw materials of the present invention is simple, Financial cost is low, prepared fluorescent material is nontoxic, be difficult for deliquescence, physicochemical property are stable, luminescent properties is convenient to control, durable in use, environmentally safe; The preparation method who provides is simple, operability is easy to control, the preparation good reproducibility, is suitable for large-scale industrialization production.Fluorescent material of the present invention is applicable to the device of making multiple illumination or indicating system, as: office lighting system, factory illumination system, lighting of home system, roadway lighting system, decorative lightening system, automobile lighting system, telltale lighting system etc.
Description of drawings
Fig. 1 is the powdery diffractometry picture of the fluorescent material that obtains of embodiment 1 provided by the invention.This powder diffraction spectrum and La
5Si
3O
12The standard card of N (JCPDS No.36-0571) coupling is fine.
Fig. 2 is the excitation spectrum of the fluorescent material that obtains of embodiment 1 provided by the invention, and this spectrum presents the wideband spectrum structure, excites approximately 340nm of peak position, and this fluorescent material can effectively be excited in the 250-450nm wavelength region.
Fig. 3 is the emmission spectrum of the fluorescent material that obtains of embodiment 1 provided by the invention, and this emmission spectrum frequency band approximately is in the 450-650nm scope, and the emission peak position is 510nm approximately.
Embodiment
Following embodiment is used for further describing the present invention, but does not limit in any form the present invention.
Raw material used in embodiment is the commercial goods.Wherein: lanthanum sesquioxide, purity＞99.99%; Silicon-dioxide, purity＞99.99%; Silicon nitride, purity＞99.99%; Europiumsesquioxide, purity＞99.99%.
Embodiment 1
Press chemical formula (La
0.95Eu
0.05)
5Si
3O
12Each element mole proportioning raw materials weighing: La in N
2O
3Powder 5.004 grams, SiO
2Powder 0.8740 gram, Si
3N
4Powder 0.2265 gram, Eu
2O
3Powder 0.2846 gram; Mix being placed in ball mill, ball milling 1 hour takes out ball-milled powder, uses the tabletting machine compressing tablet, tabletting machine pressure 15MPa, and compressing tablet thickness is 11mm approximately, diameter 13mm; Print being placed in the High Temperature High Pressure graphite furnace, fully vacuumizing, is that 95:5 passes into the nitrogen and hydrogen mixture source by the volume ratio of nitrogen and hydrogen, is warming up to 1250 ℃, heat preservation sintering 3 hours; The hydrogen source gas of breaking is sealed other gas source valves, and being filled with high pure nitrogen pressure to the stove is 0.5MPa, is warming up to 1550 ℃, heat preservation sintering 3 hours; Opening the escape pipe valve, pressure drop in stove to normal pressure, is opened the inlet pipe valve, is that 95:5 passes into the nitrogen and hydrogen mixture source by the volume ratio of nitrogen and hydrogen, under the protective atmosphere of nitrogen and hydrogen, will naturally be down to room temperature in stove; Take out press sheet compression, grind, namely get the fluorescent powder material.Survey its fluorescent powder material diffraction, excite and emmission spectrum result such as Fig. 1, Fig. 2 and shown in Figure 3.
Embodiment 2
Press chemical formula (La
0.99Eu
0.01)
5Si
3O
12Each element mole proportioning raw materials weighing: La in N
2O
3Powder 5.002 grams, SiO
2Powder 0.8385 gram, Si
3N
4Powder 0.2177 gram, Eu
2O
3Powder 0.0544 gram; Mix being placed in ball mill, ball milling 1 hour takes out ball-milled powder, uses the tabletting machine compressing tablet, tabletting machine pressure 15MPa, and compressing tablet thickness is 11mm approximately, diameter 13mm; Print being placed in the High Temperature High Pressure graphite furnace, fully vacuumizing, is that 95:5 passes into the nitrogen and hydrogen mixture source by the volume ratio of nitrogen and hydrogen, is warming up to 1250 ℃, heat preservation sintering 3 hours; The hydrogen source gas of breaking is sealed other gas source valves, and being filled with high pure nitrogen pressure to the stove is 0.5MPa, is warming up to 1450 ℃, heat preservation sintering 3 hours; Opening the escape pipe valve, pressure drop in stove to normal pressure, is opened the inlet pipe valve, is that 95:5 passes into the nitrogen and hydrogen mixture source by the volume ratio of nitrogen and hydrogen, under the protective atmosphere of nitrogen and hydrogen, will naturally be down to room temperature in stove; Take out press sheet compression, grind, namely get the fluorescent powder material.
Embodiment 3
Press chemical formula (La
0.9Eu
0.1)
5Si
3O
12Each element mole proportioning raw materials weighing: La in N
2O
3Powder 5.0002 grams, SiO
2Powder 0.9022 gram, Si
3N
4Powder 0.2390 gram, Eu
2O
3Powder 0.6000 gram; Mix being placed in ball mill, ball milling 1 hour takes out ball-milled powder, uses the tabletting machine compressing tablet, tabletting machine pressure 15MPa, and compressing tablet thickness is 11mm approximately, diameter 13mm; Print being placed in the High Temperature High Pressure graphite furnace, fully vacuumizing, is that 95:5 passes into the nitrogen and hydrogen mixture source by the volume ratio of nitrogen and hydrogen, is warming up to 1250 ℃, heat preservation sintering 3 hours; The hydrogen source gas of breaking is sealed other gas source valves, and being filled with high pure nitrogen pressure to the stove is 0.5MPa, is warming up to 1500 ℃, heat preservation sintering 3 hours; Opening the escape pipe valve, pressure drop in stove to normal pressure, is opened the inlet pipe valve, is that 95:5 passes into the nitrogen and hydrogen mixture source by the volume ratio of nitrogen and hydrogen, under the protective atmosphere of nitrogen and hydrogen, will naturally be down to room temperature in stove; Take out press sheet compression, grind, namely get the fluorescent powder material.
Embodiment 4
Press chemical formula (La
0.85Eu
0.15)
5Si
3O
12Each element mole proportioning raw materials weighing: La in N
2O
3Powder 5.003 grams, SiO
2Powder 0.9766 gram, Si
3N
4Powder 0.2532 gram, Eu
2O
3Powder 0.9533 gram; Mix being placed in ball mill, ball milling 1.5 hours takes out ball-milled powder, uses the tabletting machine compressing tablet, tabletting machine pressure 13MPa, and compressing tablet thickness is 10mm approximately, diameter 13mm; Print being placed in the High Temperature High Pressure graphite furnace, fully vacuumizing, is that 95:5 passes into the nitrogen and hydrogen mixture source by the volume ratio of nitrogen and hydrogen, is warming up to 1000 ℃, heat preservation sintering 5 hours; The hydrogen source gas of breaking is sealed other gas source valves, and being filled with high pure nitrogen pressure to the stove is 0.8MPa, is warming up to 1450 ℃, heat preservation sintering 5 hours; Opening the escape pipe valve, pressure drop in stove to normal pressure, is opened the inlet pipe valve, is that 95:5 passes into the nitrogen and hydrogen mixture source by the volume ratio of nitrogen and hydrogen, under the protective atmosphere of nitrogen and hydrogen, will naturally be down to room temperature in stove; Take out press sheet compression, grind, namely get the fluorescent powder material.
Embodiment 5
Press chemical formula (La
0.8Eu
0.2)
5Si
3O
12Each element mole proportioning raw materials weighing: La in N
2O
3Powder 5.004 grams, SiO
2Powder 1.0375 grams, Si
3N
4Powder 0.2692 gram, Eu
2O
3Powder 1.3505 grams; Mix being placed in ball mill, ball milling 2 hours takes out ball-milled powder, uses the tabletting machine compressing tablet, tabletting machine pressure 18MPa, and compressing tablet thickness is 12mm approximately, diameter 13mm; Print being placed in the High Temperature High Pressure graphite furnace, fully vacuumizing, is that 95:5 passes into the nitrogen and hydrogen mixture source by the volume ratio of nitrogen and hydrogen, is warming up to 1110 ℃, heat preservation sintering 10 hours; The hydrogen source gas of breaking is sealed other gas source valves, and being filled with high pure nitrogen pressure to the stove is 1MPa, is warming up to 1500 ℃, heat preservation sintering 3 hours; Opening the escape pipe valve, pressure drop in stove to normal pressure, is opened the inlet pipe valve, is that 95:5 passes into the nitrogen and hydrogen mixture source by the volume ratio of nitrogen and hydrogen, under the protective atmosphere of nitrogen and hydrogen, will naturally be down to room temperature in stove; Take out press sheet compression, grind, namely get the fluorescent powder material.
Embodiment 6
Press chemical formula (La
0.75Eu
0.25)
5Si
3O
12Each element mole proportioning raw materials weighing: La in N
2O
3Powder 5.003 grams, SiO
2Powder 1.1066 grams, Si
3N
4Powder 0.2872 gram, Eu
2O
3Powder 1.8001 grams; Mix being placed in ball mill, ball milling 1 hour takes out ball-milled powder, uses the tabletting machine compressing tablet, tabletting machine pressure 15MPa, and compressing tablet thickness is 11mm approximately, diameter 13mm; Print being placed in the High Temperature High Pressure graphite furnace, fully vacuumizing, is that 95:5 passes into the nitrogen and hydrogen mixture source by the volume ratio of nitrogen and hydrogen, is warming up to 1250 ℃, heat preservation sintering 3 hours; The hydrogen source gas of breaking is sealed other gas source valves, and being filled with high pure nitrogen pressure to the stove is 0.5MPa, is warming up to 1550 ℃, heat preservation sintering 3 hours; Opening the escape pipe valve, pressure drop in stove to normal pressure, is opened the inlet pipe valve, is that 95:5 passes into the nitrogen and hydrogen mixture source by the volume ratio of nitrogen and hydrogen, under the protective atmosphere of nitrogen and hydrogen, will naturally be down to room temperature in stove; Take out press sheet compression, grind, namely get the fluorescent powder material.
Claims (9)
1. an europium doping group of the lanthanides silica nitrogen compound, is characterized in that, its chemical general formula is: La
5-5xEu
5xSi
3O
12N, wherein, 0＜x＜0.25.
2. europium doping group of the lanthanides silica nitrogen compound according to claim 1, is characterized in that 0＜x in described chemical general formula＜0.1.
3. the preparation method of an europium doping group of the lanthanides silica nitrogen compound, is characterized in that, it comprises the following steps preparation:
(a) according to chemical formula La
5-5xEu
5xSi
3O
12N, wherein mole proportioning raw materials weighing of 0＜x＜0.25: lanthanum sesquioxide, silicon-dioxide, silicon nitride, europiumsesquioxide;
(b) raw material is carried out ball milling, the powder after ball milling carries out compressing tablet;
(c) compressing tablet is placed in High Temperature Furnaces Heating Apparatus, is filled with nitrogen, hydrogen mixing source of the gas in stove, furnace temperature is risen to 1000～1250 ℃, sintering 3～10 hours;
(d) turn off hydrogen source gas, under the environment that is filled with the nitrogen source of the gas, the air pressure of High Temperature Furnaces Heating Apparatus maintains under 0.5～1MPa, and furnace temperature rises to 1450～1550 ℃, and compressing tablet was continued sintering 3～10 hours;
(e) ventilation makes the pressure in High Temperature Furnaces Heating Apparatus reduce to normal pressure, under the circulation of nitrogen, hydrogen mixing source of the gas, makes High Temperature Furnaces Heating Apparatus naturally be down to room temperature, takes out compressing tablet, grinds, and namely gets fluorescent material.
4. the preparation method of europium doping group of the lanthanides silica nitrogen compound according to claim 3, is characterized in that 0＜x＜0.1 in step (a).
5. the preparation method of europium doping group of the lanthanides silica nitrogen compound according to claim 3, is characterized in that, the described Ball-milling Time of step (b) is 1～2 hour.
6. the preparation method of europium doping group of the lanthanides silica nitrogen compound according to claim 3, is characterized in that, during step (b) compressing tablet, pressure is 13～18MPa.
7. the preparation method of europium doping group of the lanthanides silica nitrogen compound according to claim 3, is characterized in that, the described sintering time of step (c) is 3 hours.
8. the preparation method of europium doping group of the lanthanides silica nitrogen compound according to claim 3, is characterized in that, the described sintering time of step (d) is 3 hours.
9. the preparation method of europium doping group of the lanthanides silica nitrogen compound according to claim 3, is characterized in that, the air pressure of the described High Temperature Furnaces Heating Apparatus of step (d) is at 0.5MPa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104927858A (en) * | 2015-07-02 | 2015-09-23 | 河北大学 | Nitride fluorescent material capable of emitting green light under excitation of blue light as well as preparation method and application thereof |
| CN105441078A (en) * | 2014-09-30 | 2016-03-30 | 中国科学院上海硅酸盐研究所 | Rare earth ion Eu<2+>-doped Y5Si3O12N fluorescent powder and preparation method therefor |
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| CN102559184A (en) * | 2011-12-31 | 2012-07-11 | 河北大学 | Silicon-based nitrogen oxide fluorescent powder and preparation method thereof |
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- 2013-03-15 CN CN201310082631.8A patent/CN103146386B/en not_active Expired - Fee Related
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| US20110163322A1 (en) * | 2009-08-10 | 2011-07-07 | Jae Soo Yoo | Phosphor, phosphor manufacturing method, and white light emitting device |
| CN102559184A (en) * | 2011-12-31 | 2012-07-11 | 河北大学 | Silicon-based nitrogen oxide fluorescent powder and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105441078A (en) * | 2014-09-30 | 2016-03-30 | 中国科学院上海硅酸盐研究所 | Rare earth ion Eu<2+>-doped Y5Si3O12N fluorescent powder and preparation method therefor |
| CN105441078B (en) * | 2014-09-30 | 2017-07-14 | 中国科学院上海硅酸盐研究所 | Rare earth ion Eu2+The Y of doping5Si3O12N fluorescent material and preparation method thereof |
| CN104927858A (en) * | 2015-07-02 | 2015-09-23 | 河北大学 | Nitride fluorescent material capable of emitting green light under excitation of blue light as well as preparation method and application thereof |
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