CN102952542B - Nitride or nitrogen oxide fluorescent powder and preparation method thereof - Google Patents

Nitride or nitrogen oxide fluorescent powder and preparation method thereof Download PDF

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CN102952542B
CN102952542B CN201210410417.6A CN201210410417A CN102952542B CN 102952542 B CN102952542 B CN 102952542B CN 201210410417 A CN201210410417 A CN 201210410417A CN 102952542 B CN102952542 B CN 102952542B
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nitride
fluorescent powder
roasting
oxide fluorescent
nitric oxide
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CN102952542A (en
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何锦华
滕晓明
梁超
符义兵
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Jiangsu Borui Photoelectric Co ltd
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JIANGSU BREE OPTRONICS CO Ltd
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Abstract

The invention discloses a method for manufacturing nitride or oxynitride fluorescent powder, which comprises the following steps: a. weighing required raw materials in Ca, Sr or Al nitride, Si nitride or oxide or barium carbonate according to the stoichiometric ratio of a target product, and uniformly mixing the raw materials with europium oxide and SiC, wherein the molar amount of the europium oxide is 0.1-30% of the molar amount of the raw materials, and the mass amount of the SiC is 1-5wt% of the mass of the raw materials; b. b, carrying out anaerobic roasting on the material obtained in the step a; c. and d, cooling the material obtained in the step b to obtain the nitride or nitrogen oxide fluorescent powder. The preparation method of the nitride or nitrogen oxide fluorescent powder prevents Si3N4The excessive growth of crystal grains, the refinement of the crystal grain structure and the reduction of the grain diameter of the product, the narrower grain diameter distribution, the proper grain diameter of the synthesized nitride or nitrogen oxide fluorescent powder, the direct application without ball milling, and the improvement of the anti-aging performance of the nitride or nitrogen oxide fluorescent powder; the crystallinity of the product is increased, and the fluorescence property is higher;the sintering temperature in the roasting process is reduced, and the sintering time is reduced.

Description

A kind of nitride or nitric oxide fluorescent powder and preparation method thereof
Technical field
The present invention relates to a kind of nitride or nitric oxide fluorescent powder and preparation method thereof.
Background technology
As the 4th generation lighting source LED, in the implementation of present stage, fluorescent material is in occupation of consequence.It is through development for many years, the plurality of advantages such as nitride and nitric oxide fluorescent powder were found to have in recent years high luminous efficiency, can be effectively excited by ultraviolet and visible ray, spectral response curve designability is strong, thermostability is high and physical and chemical performance is stable, therefore, carried out a large amount of research work and obtained the nitride/nitric oxide fluorescent powder of various new in this direction.But nitride/nitric oxide fluorescent powder is due to its inherent physico-chemical property, its synthesis condition harshness, particle size were is large and inhomogeneous, for reaching application requiring, also needs to carry out aftertreatment.
Technology contents
The invention provides a kind of nitride or nitric oxide fluorescent powder and preparation method thereof.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A manufacture method for nitride or nitric oxide fluorescent powder, comprises the steps:
A, in the nitride or oxide compound or barium carbonate of the nitride of Ca, Sr or Al, Si, according to target the stoichiometric ratio of product takes desired raw material, mix with europium sesquioxide and SiC, the mole dosage of described europium sesquioxide is the 0.1%-30% of feed molar number, the 1-5wt% that the quality consumption of described SiC is raw materials quality;
B, by the roasting of step a gained material anaerobic;
C, by cooling step b gained material, obtain nitride or nitric oxide fluorescent powder.
Above-mentioned stoichiometric ratio refers to the stoichiometric ratio of target product.Adding of above-mentioned SiC has unexpected effect to the lifting of product performance, is applicable to the preparation of any nitride or nitric oxide fluorescent powder.
In order to ensure the homogeneity of roasting, in step a, mix as mixing by ratio of grinding media to material 1:2 in glove box.
In order to improve the performance of nitride or nitric oxide fluorescent powder, the particle diameter of described SiC is 10-50nm.
In above-mentioned steps b, roasting condition when anaerobic roasting can be prepared with reference to nitride in prior art or nitric oxide fluorescent powder.
For further stopping the existence of oxygen, reduce the nitrogen loss in material in roasting process, in step b simultaneously; before anaerobic roasting; first roasting system is vacuumized, then pass into shielding gas to normal pressure, described shielding gas is the mixed gas that nitrogen or hydrogen and nitrogen volume ratio are 5:95-75:25.When roasting, step a gained material can be packed in alumina crucible or molybdenum crucible, put into tube furnace, before roasting, with vaccum-pumping equipment, burner hearth be carried out to deoxygenation, then pass into shielding gas to normal pressure.Vaccum-pumping equipment comprises mechanical pump, diffusion pump, lobe pump or molecular pump.
In order further to improve the performance of nitride or nitric oxide fluorescent powder, in step c, after cooling step b gained material, cross 300-400 mesh sieve, and wash to specific conductivity and be less than after 10 μ s/cm, dry, obtain nitride or nitric oxide fluorescent powder.
Nitride after above-mentioned 300-400 mesh sieve excessively or the actual particle size of nitric oxide fluorescent powder are 8-10 μ m.
In order further to improve the performance of nitride or nitric oxide fluorescent powder, above-mentioned washing is that the material after sieving is immersed in the salpeter solution of 5-10%, stirs 20-30min, then is less than 10 μ s/cm by deionized water wash to specific conductivity.The object that nitric acid is washed is for the impurity in nitride or nitric oxide fluorescent powder is effectively dissolved, and then removes.
In order to ensure drying efficiency, do not affect product performance simultaneously, described oven dry is at 80-100 DEG C, dries 3-5h.Oven dry can be carried out in air blast bellows.
In order to improve the performance of nitride or nitric oxide fluorescent powder; in above-mentioned steps b; anaerobic roasting is: under shielding gas; constant-pressure and high-temperature solid phase baking inphases; comprise the steps: first paragraph roasting; temperature rise rate is 15-20 DEG C/min; shield gas flow rate is 0.1-0.5L/min; target temperature is 700-1100 ° of C, and under target temperature, roasting time is 2-5h, second segment roasting; temperature rise rate is 5-10 DEG C/min; shield gas flow rate is 0.1-0.5L/min, and target temperature is 1500-2000 DEG C, and under target temperature, roasting time is 8-20h.
By the prepared nitride of above-mentioned method or nitric oxide fluorescent powder, its particle diameter is 8-10 μ m.
The preparation method of nitride of the present invention or nitric oxide fluorescent powder, has stoped Si 3n 4the hypertrophy of crystal grain, crystal grain thinning tissue, reduces particle size were, and size distribution is narrower, synthetic nitride or nitric oxide fluorescent powder particle diameter are suitable, just can directly apply without ball milling, are conducive to improve the ageing resistance of nitride or nitric oxide fluorescent powder; The degree of crystallinity that has increased product, fluorescence property is higher; Reduce the sintering temperature in roasting process, while having reduced sintering; Manufacture method is simple, and easy handling is pollution-free, and cost is low; Gained nitride or nitric oxide fluorescent powder can effectively be excited by ultraviolet, purple light or blue light, send and have the fluorescence that peak wavelength is 600-750nm scope.
Brief description of the drawings
Fig. 1 is the utilizing emitted light spectrogram of embodiment 1 and comparative example 1.
Fig. 2 is the XRD figure of embodiment 1 and comparative example 1.
Fig. 3 is the ageing resistance comparison of embodiment 1 and comparative example 1
Fig. 4 is the utilizing emitted light spectrogram of embodiment 2 and comparative example 2.
Fig. 5 is embodiment 2(a) and the SEM figure of comparative example 2 (b).
Fig. 6 is the utilizing emitted light spectrogram of embodiment 3 and comparative example 3.
Fig. 7 is the particle size distribution figure of embodiment 3 and comparative example 3.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1
(1) take Ca 3n 26.671g, Si 3n 46.575g, AlN5.764g, Eu 2o 30.99g, 10nmSiC0.20g fully mixes above raw material by ratio of grinding media to material 1:2 in glove box, packs in molybdenum crucible;
(2) molybdenum crucible is moved into rapidly in tube furnace, then use respectively mechanical pump, lobe pump and diffusion pump to carry out deoxygenation to burner hearth;
(3), under the protection of normal pressure, pure nitrogen gas atmosphere, be warming up to gradually 900 DEG C with the speed of 18 DEG C/min, insulation 3h, gas flow is 0.2L/min, then, under the protection of the mixed atmosphere of nitrogen hydrogen, is warming up to gradually 1750 DEG C with the speed of 8 DEG C/min, insulation 15h, total gas flow rate is 0.3L/min;
(4) direct mistake 300 eye mesh screens of synthetic fluorescent material, then in 6% salpeter solution, stir 30min, then with deionized water wash to specific conductivity be 8.2 μ s/cm, then in the convection oven of 90 DEG C, dry 3h, can make Ca 0.96alSiN 3: the Nitride phosphor of 0.04Eu.
Gained fluorescent material and YAG fluorescent material and blue chip combination, through encapsulation burn-in test, within 1000 hours, light decay is 2.2%.
Comparative example 1
(1) take Ca 3n 26.671g, Si 3n 46.575g, AlN5.764g, Eu 2o 30.99g fully mixes above raw material by ratio of grinding media to material 1:2 in glove box, packs in molybdenum crucible;
(2) molybdenum crucible is moved into rapidly in tube furnace, then use respectively mechanical pump, lobe pump and diffusion pump to carry out deoxygenation to burner hearth;
(3), under the protection of normal pressure, pure nitrogen gas atmosphere, be warming up to gradually 900 DEG C with the speed of 18 DEG C/min, insulation 3h, gas flow is 0.2L/min, then, under the protection of the mixed atmosphere of nitrogen hydrogen, is warming up to gradually 1750 DEG C with the speed of 8 DEG C/min, insulation 15h, total gas flow rate is 0.3L/min;
(4) the first ball milling of synthetic fluorescent material, then crosses 300 eye mesh screens, then, in 6% salpeter solution, stirs 30min, then with deionized water wash to specific conductivity be 8.2 μ s/cm, then in the convection oven of 90 DEG C, dry 3h, can make Ca 0.96alSiN 3: the Nitride phosphor of 0.04Eu.
Gained fluorescent material and YAG fluorescent material and blue chip combination, through encapsulation burn-in test, within 1000 hours, light decay is 4.5%.
Embodiment 2
(1) take Sr 3n 28.76g, Si 3n 410.833g, Eu 2o 30.408g, 50nmSiC1.0g fully mixes above raw material by ratio of grinding media to material 1:2 in glove box, packs in molybdenum crucible;
(2) molybdenum crucible is moved into rapidly in tube furnace, then use respectively mechanical pump, lobe pump and molecular pump to carry out deoxygenation to burner hearth;
(3), under the protection of normal pressure, pure nitrogen gas atmosphere, be warming up to gradually 800 DEG C with the speed of 15 DEG C/min, insulation 4h, gas flow is 0.3L/min, then, under the protection of the mixed atmosphere of nitrogen hydrogen, is warming up to gradually 1550 DEG C with the speed of 9 DEG C/min, insulation 10h, total gas flow rate is 0.5L/min;
(4) direct mistake 400 eye mesh screens of synthetic fluorescent material, then in 5% salpeter solution, stir 30min, then with deionized water wash to specific conductivity be 4.3 μ s/cm, then in the convection oven of 80 DEG C, dry 5h, can make Sr 1.95si 5n 8: the Nitride phosphor of 0.05Eu.
Gained fluorescent material and YAG fluorescent material and blue chip combination, through encapsulation burn-in test, within 1000 hours, light decay is 8.8%.
Comparative example 2
(1) take Sr 3n 28.76g, Si 3n 410.833g, Eu 2o 30.408g fully mixes above raw material by ratio of grinding media to material 1:2 in glove box, packs in molybdenum crucible;
(2) molybdenum crucible is moved into rapidly in tube furnace, then use respectively mechanical pump, lobe pump and molecular pump to carry out deoxygenation to burner hearth;
(3), under the protection of normal pressure, pure nitrogen gas atmosphere, be warming up to gradually 800 DEG C with the speed of 15 DEG C/min, insulation 4h, gas flow is 0.3L/min, then, under the protection of the mixed atmosphere of nitrogen hydrogen, is warming up to gradually 1550 DEG C with the speed of 9 DEG C/min, insulation 10h, total gas flow rate is 0.5L/min;
(4) the first ball milling of synthetic fluorescent material, then crosses 400 eye mesh screens, then, in 5% salpeter solution, stirs 30min, then with deionized water wash to specific conductivity be 4.3 μ s/cm, then in the convection oven of 80 DEG C, dry 5h, can make Sr 1.95si 5n 8: the Nitride phosphor of 0.05Eu.
Gained fluorescent material and YAG fluorescent material and blue chip combination, through encapsulation burn-in test, within 1000 hours, light decay is 12.5%.
Embodiment 3
(1) take BaCO 312.525g, SiO 21.907g, Si 3n 44.452g, Eu 2o 31.117g, 25nmSiC0.50g fully mixes above raw material by ratio of grinding media to material 1:2 in glove box, packs in alumina crucible;
(2) alumina crucible is moved into rapidly in tube furnace, then use respectively mechanical pump and lobe pump to carry out deoxygenation to burner hearth;
(3) under the protection of normal pressure, pure nitrogen gas atmosphere, be warming up to gradually 1100 DEG C with the speed of 20 DEG C/min, insulation 2h, gas flow is 0.1L/min, then, under the protection of the mixed atmosphere of nitrogen hydrogen, is warming up to gradually 1350 DEG C with the speed of 6 DEG C/min, insulation 8h, total gas flow rate is 0.4L/min;
(4) direct mistake 300 eye mesh screens of synthetic fluorescent material, then in 8% salpeter solution, stir 30min, then with deionized water wash to specific conductivity be 6.7 μ s/cm, then in the convection oven of 100 DEG C, dry 4h, can make Ba 0.9si 2o 2n 2: the Nitride phosphor of 0.1Eu.
Gained fluorescent material and YAG fluorescent material and blue chip combination, through encapsulation burn-in test, within 1000 hours, light decay is 7.6%.
Comparative example 3
(1) take BaCO 312.525g, SiO 21.907g, Si 3n 44.452g, Eu 2o 31.117g fully mixes above raw material by ratio of grinding media to material 1:2 in glove box, packs in alumina crucible;
(2) alumina crucible is moved into rapidly in tube furnace, then use respectively mechanical pump and lobe pump to carry out deoxygenation to burner hearth;
(3) under the protection of normal pressure, pure nitrogen gas atmosphere, be warming up to gradually 1100 DEG C with the speed of 20 DEG C/min, insulation 2h, gas flow is 0.1L/min, then, under the protection of the mixed atmosphere of nitrogen hydrogen, is warming up to gradually 1350 DEG C with the speed of 6 DEG C/min, insulation 8h, total gas flow rate is 0.4L/min;
(4) the first ball milling of synthetic fluorescent material, then crosses 300 eye mesh screens, then, in 8% salpeter solution, stirs 30min, then with deionized water wash to specific conductivity be 6.7 μ s/cm, then in the convection oven of 100 DEG C, dry 4h, can make Ba 0.9si 2o 2n 2: the Nitride phosphor of 0.1Eu.
Gained fluorescent material and YAG fluorescent material and blue chip combination, through encapsulation burn-in test, within 1000 hours, light decay is 10.8%.

Claims (9)

1. a manufacture method for nitride or nitric oxide fluorescent powder, is characterized in that: comprise the steps:
A, in A, B or C, according to target the stoichiometric ratio of product takes desired raw material, mix with europium sesquioxide and SiC, the mole dosage of described europium sesquioxide is the 0.1%-30% of feed molar number, the 1-5wt% that the quality consumption of described SiC is raw materials quality, wherein, A is the nitride of Ca, Sr or Al, B is nitride or the oxide compound of Si, and C is barium carbonate;
B, by the roasting of step a gained material anaerobic;
C, by cooling step b gained material, obtain nitride or nitric oxide fluorescent powder;
In step a, the particle diameter of described SiC is 10-50nm.
2. the method for claim 1, is characterized in that: in step c, after cooling step b gained material, cross 300-400 mesh sieve, and wash to specific conductivity and be less than after 10 μ s/cm, dry, obtain nitride or nitric oxide fluorescent powder.
3. method as claimed in claim 2, is characterized in that: described washing is that the material after sieving is immersed in the salpeter solution of 5-10%, stirs 20-30min, then is less than 10 μ s/cm by deionized water wash to specific conductivity.
4. method as claimed in claim 2, is characterized in that: described oven dry is at 80-100 DEG C, dries 3-5h.
5. the method as described in claim 1 to 4 any one, is characterized in that: in step a, mix as mixing by ratio of grinding media to material 1:2 in glove box.
6. the method as described in claim 1 to 4 any one; it is characterized in that: in step b, before anaerobic roasting, first roasting system is vacuumized; then pass into shielding gas to normal pressure, described shielding gas is the mixed gas that nitrogen or hydrogen and nitrogen volume ratio are 5:95-75:25.
7. method as claimed in claim 6; it is characterized in that: in described step b; anaerobic roasting is: under shielding gas; constant-pressure and high-temperature solid phase baking inphases; comprise the steps: first paragraph roasting; temperature rise rate is 15-20 DEG C/min; shield gas flow rate is 0.1-0.5L/min; target temperature is 700-1100 DEG C, and under target temperature, roasting time is 2-5h, second segment roasting; temperature rise rate is 5-10 DEG C/min; shield gas flow rate is 0.1-0.5L/min, and target temperature is 1500-2000 DEG C, and under target temperature, roasting time is 8-20h.
8. by the method described in claim 1 to 7 any one prepared nitride or nitric oxide fluorescent powder.
9. nitride as claimed in claim 8 or nitric oxide fluorescent powder, is characterized in that: its particle diameter is 8-10 μ m.
CN201210410417.6A 2012-10-24 2012-10-24 Nitride or nitrogen oxide fluorescent powder and preparation method thereof Active CN102952542B (en)

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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
CN105733571A (en) * 2016-01-29 2016-07-06 江苏博睿光电有限公司 Nitric oxide luminous particle and preparation method thereof, nitric oxide luminous body and luminous device

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