CN103173214A - Synthesizing method of spherical silicon-based nitrogen compound fluorescent material - Google Patents
Synthesizing method of spherical silicon-based nitrogen compound fluorescent material Download PDFInfo
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- CN103173214A CN103173214A CN2013100710858A CN201310071085A CN103173214A CN 103173214 A CN103173214 A CN 103173214A CN 2013100710858 A CN2013100710858 A CN 2013100710858A CN 201310071085 A CN201310071085 A CN 201310071085A CN 103173214 A CN103173214 A CN 103173214A
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Abstract
The invention disclose a synthesizing method of a spherical silicon-based nitrogen compound fluorescent material. The method comprises the steps that: Alkaline earth metal and rare earth metal are subjected to ammoniation dissolution; ammoniated metal is uniformly mixed with spherical amorphous Si3+xN4-x; the uniformly mixed reaction material is added into a nitrogen-purged synthesis furnace, such that a synthesis product is obtained; the treated product is cooled to 800 DEG C with a speed of 10 DEG C/min; heating electricity is shut down, and nitrogen filling is continued, such that a pressure of 0.1Mpa is maintained in the furnace; the product is cooled to normal temperature with the furnace; nitrogen filling is stopped, and the synthesis product is fetched. According to the invention, the spherical active amorphous Si3+xN4-x powder is used for substituting a traditional silicon nitride precursor. On the basis, with a precursor component fine composition process and normal-temperature and low-temperature synthesis technical route, the spherical characterized product is obtained. Therefore, silicon-based nitride fluorescent powder luminescent property optimal development is realized, and subsequent coating operations are simple and feasible. Therefore, product cost is reduced, and product quality is improved.
Description
Technical field
The present invention relates to rare earth silicon based compound fluorescent material synthetic method, especially relate to the synthetic method of a kind of spherical silica-based nitrogen compound fluorescent material that the LED lighting source uses.
Background technology
The silicon base compound fluorescent material, because crystalline structure is by SiX (X=O, N) covalent linkage forms the tetrahedral network structure feature, makes it to have very high chemical stability and spectrum thermostability, is the key base mateiral of LED device to the high-power type development.In the silicon base compound fluorescent material structure, rich nitrogen crystal field environment causes the nephelauxetic effect that rare earth activation ion is larger, make rare earth ion 5d electron excitation energy level reduce, impel fluorescence excitation and the emission of fluorescent material to the long wave direction, can efficiently be excited, launch by blue light or near-ultraviolet light, be complementary and form warm white type spectrum with blue light, obtain the colour temperature close with daylight, make the illuminated object color pure undistorted, be suitable for the white light source as interior lighting, lighting for medical use, meet the energy-saving and environmental protection technical requirements that the mankind propose the Novel electric light source.
Need to obtain the material of the primitive reaction unit such as N source and Si source in silica-based nitrogen compound forming process, at first nineteen ninety-five Schlieper research group opens up Si (NH
2)
2, alkaline-earth metal, rare-earth europium be the synthetic M of raw material
2si
5n
8(M=Ca, Ba, Sr), its excellent luminescent properties causes scientific and technological circle's extensive concern, but Si (NH
2)
2very easily oxidation moisture absorption, prepare special, preservation difficulty, is difficult to apply in suitability for industrialized production; Li subsequently, Y. Q., Machida, Piao, the investigators such as X. are with Si
3n
4replace Si (NH
2)
2, take the technology such as two-step approach, carbothermic method or gas phase reduction process synthetic, but two step synthesis excessive cycle, carbothermic method Residual reactants and generation by product are difficult to effective the separation, greatly affect the luminescent properties of material; And Si
3n
4the strong covalent bond characteristic, cause that the starting raw material self-diffusion coefficient is low, reactive behavior is low, need higher synthesis temperature (1500～2000 ℃), long-time insulation, high temperature is synthetic particle aggregation, thick (the 8-10 μ m) caused for a long time, size distribution is uneven, need ball mill crushing to process just can be suitable for the later stage coating processes, and the impurity that break process is brought and dephasign have greatly affected its luminescent properties, and this problem is not yet effectively solved up till now.European patent EP 2163593 A1 disclose with Eu[N(Si(CH
3)
3)
2]
3, SiCl
4for raw material, utilize alkaline-earth metal can be dissolved in the characteristics of liquefied ammonia, in ammonia solvent, by wet chemistry method synthesis of silica-base nitride, its reactional equation is:
(2-?x)?M?+?xEu?[N?(Si?(CH3)
3)
2]
3?+?5SiCl
4?+?30NH
3
→?M
2-xEuxSi
5N
8?+?20?NH
4Cl?+?N
2?+?(5-1.5x)?H
2?+3xNH(Si(CH
3)
3)
2
But a large amount of organic and inorganic by product serious environment pollution that the method forms.
Summary of the invention
The object of the present invention is to provide a kind of synthetic method of spherical silica-based nitrogen compound fluorescent material, when changing synthesis condition maintenance material luminescent properties, improve the micromeritis performance of material.
The technical solution used in the present invention is:
Adopt the synthetic acquisition of vapor phase process spherical, be evenly distributed, the certain active nitrogenous non-crystalline silicon (Si of band
3+xn
4-x) be the original presoma of matrix, utilize the chemically reactive that matrix is nitrogenous and amorphous brings, alkaline-earth metal can form the characteristic of ammino metallic solution, by liquid phase wet chemistry method composite fine metal on the nitrogenous non-crystalline silicon of matrix, guarantee that metal evenly mixes with the matrix non-crystalline silicon, improve material mutual diffusion performance in granular precursor, accelerate solid phase synthesis speed, reduce synthesis temperature, time, retained the good micromeritis characteristic of matrix presoma simultaneously, and acquisition powder degree of crystallinity, crystalline phase, impurity phase content, granule-morphology, size-grade distribution, the silica-based nitride fluorescent material that the micromeritis characteristic conforms such as dispersiveness require, realize the simple and feasible of the best performance of its luminescent properties and later stage coat operations, when reducing product cost, improve the quality of products.
The selected matrix of the present invention is the synthetic amorphous Si of vapor phase process
3+xn
4-x, its building-up process is as follows:
SiH
4?+?NH
3?→?Si
3+xN
4-x?+H
2
Granularity is 0.2-2 μ, wherein preferably spherical, the active amorphous state Si of 0.5-1 μ
3+xn
4-xfor the Si source.Utilize on the other hand alkaline-earth metal and rare earth metal can be dissolved in the characteristics that liquefied ammonia forms the ammonification metal, both avoided the problem of oxidation of alkaline-earth metal, can in ammonia solvent, realize that again alkaline earth dilution metal is with active amorphous state Si
3+xn
4-xthe purpose of evenly mixing between atom, the selected alkaline-earth metal of the present invention be-a kind of in Ш main group element Li, K, Na, Mg, Ca, Sr, Ba, B, Al, Ga or two kinds, a kind of in preferred Li, Ca, Ba, Sr, Al or two kinds; The selected rare earth metal of the present invention is one or more in Y, La, Ce, Sm, Eu, Yb, preferably Y, Eu, Yb.By spherical amorphous Si
3+xn
4-xwith the liquid ammonia solution uniform stirring of alkaline-earth metal, rare earth metal, make metal be dispersed in active spherical amorphous Si
3+xn
4-xsurface, the reactant that the slow evaporation ammonia solvent obtains all mixing while stirring, under the normal pressure nitrogen atmosphere, 1100 ℃-1400 ℃, wherein preferably silica-based nitrides are synthesized in 1200 ℃ of-1380 ℃ of nitrogenize, below the fusing point of synthesis temperature in Pure Silicon Metal, with the pattern of guaranteeing synthetics, keep spherical silicon pattern and size.The concrete steps of the method are as follows:
1) ammonification of alkaline-earth metal and rare earth metal is dissolved:
Mole ratio according to each component of silica-based nitride, in mixing equipment, under normal temperature, high pure nitrogen condition, put into 0.02mol alkaline-earth metal and rare earth metal in the container cleaned up, the alkaline-earth metal that its mole number ratio is 199:1 ~ 4:1 and rare earth metal are dissolved in the dry liquefied ammonia solvent of 100ml ~ 200ml, stirring makes dissolving metal, forms solution ammonification metal, stand-by;
2) the ammonification metal is with spherical amorphous Si
3+xn
4-xevenly mix:
Take the spherical amorphous Si of activity of 1.4g by the component mole number ratio of silica-based nitride
3+xn
4-xpowder, by above-mentioned steps 1) in 100ml ~ 200ml solution ammonification metal be added to active spherical amorphous Si
3+xn
4-xin powder, stir the solvent liquefied ammonia volatilization made in solution ammonification metal, the ammonification metal is with M (NH
3)
xthe form supersaturation separate out, and be adsorbed on spherical amorphous Si
3+xn
4-xpowder surface, form intergranular precipitation at the spherical amorphous Si of activity
3+xn
4-xon powder, realize evenly mixing, obtain all mixed reactants of design requirements;
3) by above-mentioned steps 2) all mixed reactant pack in the synthetic furnace of nitrogen purging, the high-purity N that through-flow speed is 150-200ml/min
2, keeping the stove internal gas pressure is normal pressure, with 5 ℃/min, is warmed up to 1200-1380 ℃, insulation 4-10 hour, obtain synthetic product;
4) by above-mentioned steps 3) product after processing cools to 800 ℃ with 10 ℃/min, cuts off and adds thermoelectricity, continues to fill nitrogen and makes in stove to keep 0.1Mpa pressure, and furnace cooling, to normal temperature, stops filling nitrogen, the taking-up synthetic product.
Described mixing equipment is the atmosphere protection glove box; Described synthetic furnace is the graphite heating synthesis device.
The high-purity N that described nitrogen source of the gas is 99.99%
2; Described liquefied ammonia solvent is purity 99,99%, through the CaO drying treatment liquefied ammonia that dewaters.
The beneficial effect that the present invention has is:
The present invention is with spherical active amorphous Si
3+xn
4-xpowder replaces silicon nitride precursor body in the past, passes through on this basis the synthetic technology route of the meticulous recombining process of presoma component and normal pressure, lesser temps.Obtain spherical characteristic product, realize the simple and feasible of the best performance of silica-based nitride light-emitting phosphor performance and later stage coat operations, improve the quality of products when reducing product cost.
The accompanying drawing explanation
Fig. 1 is synthetic product Ca
2si
5n
8: the SEM pattern of Eu.
Fig. 2 is synthetic product Ca
2si
5n
8: the PL spectrogram of Eu.
Embodiment
1) ammonification of alkaline-earth metal and rare earth metal is dissolved:
Under normal temperature condition, in nitrogen atmosphere, by calcium metal 0.796g and the Rare Earth Europium 0.0152g of packing in the beaker cleaned up, slowly add 100ml drying liquefied ammonia, stir and make dissolving metal, form bluish-green ammonification metallic solution, stand-by.
2) the ammonification metal evenly mixes with the amorphous nitrogenated silicon:
Component mole number ratio by synthetic product takes the spherical amorphous Si of 1.4g
3+xn
4-xpowder, by above-mentioned steps 1) form bluish-green ammonification metallic solution and slowly join amorphous Si
3+xn
4-xin powder, stir and accelerate the ammonia solvent volatilization, realize spherical amorphous Si
3+xn
4-evenly mix with the ammonification metal, obtain all mixed reactants.
3) by above-mentioned steps 2) all mixed reactant pack in crucible, advance the synthetic furnace through nitrogen purging, and the through-flow speed high-purity N that is 150/min
2, keeping the stove internal gas pressure is normal pressure, with 5 ℃/min, is warmed up to 1380 ℃, insulation 4h, obtain synthetic product.
4) by above-mentioned steps 3) product after processing cools to 800 ℃ with 10 ℃/min, cuts off and adds thermoelectricity, continues to fill nitrogen, and furnace cooling, to normal temperature, takes out synthetic product, carries out product morphology observation (as shown in Figure 1) and luminescent properties and tests (as shown in Figure 2).
Embodiment 2
1) ammonification of alkaline-earth metal and rare earth metal is dissolved:
Under normal temperature condition, in nitrogen atmosphere, in the beaker cleaned up, pack into calcium metal 0.64g and Rare Earth Europium 0.608g, the liquefied ammonia that slowly adds 100ml to dewater through CaO, stir and make dissolving metal, forms bluish-green ammonification metallic solution, stand-by.
2) the ammonification metal evenly mixes with non-crystalline silicon:
Component mole number ratio by synthetic product takes 1.4g amorphous Si
3+xn
4-xpowder, by above-mentioned steps 1) the ammonification metallic solution that forms joins amorphous Si
3+xn
4-xin powder, stir, make amorphous Si
3+xn
4-xeven with the ammonification metal mixed, accelerate the volatilization of solvent liquefied ammonia simultaneously, obtain all mixing reactant.
3) by above-mentioned steps 2) all mixed reactant pack in crucible, advance synthetic furnace, and the through-flow speed high-purity N that is 200/min
2, keeping the stove internal gas pressure is normal pressure, with 5 ℃/min, is warmed up to 1200 ℃, insulation 10h, obtain synthetic product.
4) by above-mentioned steps 3) product after processing cools to 800 ℃ with 10 ℃/min, cuts off and adds thermoelectricity, continues to fill nitrogen, and furnace cooling, to normal temperature, takes out synthetic product, carries out product morphology observation and luminescent properties and tests.
Embodiment 3
1) ammonification of alkaline-earth metal and rare earth metal is dissolved:
Under normal temperature condition, in nitrogen atmosphere, the Preparation of Metallic Strontium of packing in cleaning up beaker 1.7512g and Rare Earth Europium 0.0152g, the dry liquefied ammonia that slowly adds 150ml to dewater through CaO, stir and make dissolving metal, forms bluish-green ammonification metallic solution, stand-by.
2) the ammonification metal evenly mixes with the amorphous nitrogenated silicon:
Component mole number ratio by synthetic product takes the nitrogenous silica flour of 1.4g amorphous, by above-mentioned steps 1) in the nitrogenous silica flour of amorphous be poured in the nitrogenous silica flour beaker of amorphous, stir, make spherical amorphous Si
3+xn
4-even with the ammonification metal mixed, accelerated solvent liquefied ammonia volatilization simultaneously, obtain all mixed reactants.
3) by above-mentioned steps 2) all mixed reactant pack in crucible, advance in the synthetic furnace of nitrogen purging, and the through-flow speed high-purity N that is 150/min
2, keeping the stove internal gas pressure is normal pressure, with 5 ℃/min, is warmed up to 1350 ℃, insulation 4h obtains synthetic product.
4) by above-mentioned steps 3) product after processing cools to 800 ℃ with 10 ℃/min, cuts off and adds thermoelectricity, continues to fill nitrogen, and furnace cooling, to normal temperature, takes out synthetic product, carries out product morphology observation and luminescent properties and tests.
Embodiment 4
1) ammonification of alkaline-earth metal and rare earth metal is dissolved:
Under normal temperature condition, in nitrogen atmosphere, the Preparation of Metallic Strontium of packing in the container cleaned up 1.408g and Rare Earth Europium 0.608g, sealing, be filled with 150ml liquefied ammonia, stirs and make dissolving metal, forms bluish-green ammonification metallic solution, stand-by.
2) the ammonification metal evenly mixes with non-crystalline silicon:
Component mole number ratio by synthetic product takes the spherical amorphous Si of 1.4g
3+xn
4-xpowder, the ammonification metallic solution that above-mentioned steps 1 is formed joins amorphous Si
3+xn
4-xin powder, stir, make spherical amorphous Si
3+xn
4-powder and ammonification metal mixed are even, accelerate the volatilization of solvent liquefied ammonia, obtain all mixing reactant.
3) by above-mentioned steps 2) all mixed reactant pack in crucible, advance the synthetic furnace through nitrogen purging, and the through-flow speed high-purity N that is 200/min
2, keeping the stove internal gas pressure is normal pressure, with 5 ℃/min, is warmed up to 1200 ℃, insulation 7h obtains synthetic product.
4) by above-mentioned steps 3) product after processing cools to 800 ℃ with 10 ℃/min, cuts off and adds thermoelectricity, continues to fill nitrogen, and furnace cooling, to normal temperature, takes out synthetic product, carries out product morphology observation and luminescent properties and tests.
Embodiment 5
1) ammonification of alkaline-earth metal and rare earth metal is dissolved:
Under normal temperature condition, in nitrogen atmosphere, by barium metal 2.7263g and the Rare Earth Europium 0.0152g of packing in the high pressure vessel cleaned up, be filled with 200ml liquefied ammonia, stir and make dissolving metal, form bluish-green ammonification metallic solution, stand-by.
2) the ammonification metal evenly mixes with non-crystalline silicon:
Component mole number ratio by synthetic product takes the spherical amorphous Si of 1.4g
3+xn
4-powder, by above-mentioned steps 1) the ammonification metallic solution that forms joins spherical amorphous Si
3+xn
4-in powder, stir, make spherical amorphous Si
3+xn
4-even with the ammonification metal mixed, accelerate the volatilization of solvent liquefied ammonia, obtain all mixed reactants.
3) by above-mentioned steps 2) all mixed reactant pack in crucible, advance through the nitrogen purging synthetic furnace, and the through-flow speed high-purity N that is 150/min
2, keeping the stove internal gas pressure is normal pressure, with 5 ℃/min, is warmed up to 1350 ℃, insulation 4h obtains synthetic product.
4) by above-mentioned steps 3) product after processing cools to 800 ℃ with 10 ℃/min, cuts off and adds thermoelectricity, continues to fill nitrogen, and furnace cooling, to normal temperature, takes out synthetic product, carries out product morphology observation and luminescent properties and tests.
Embodiment 6
1) ammonification of alkaline-earth metal and rare earth metal is dissolved:
Under normal temperature condition, in nitrogen atmosphere, by barium metal 2.192g and the Rare Earth Europium 0.608g of packing in the container cleaned up, be filled with 100ml liquefied ammonia, stir and make dissolving metal, form bluish-green ammonification metallic solution, stand-by.
2) the ammonification metal is with spherical amorphous Si
3+xn
4-evenly mix:
Component mole number ratio by synthetic product takes the nitrogenous silica flour of 1.4g amorphous, by above-mentioned steps 1) in the ammonification metallic solution join in the nitrogenous silica flour of amorphous, stir, make spherical amorphous Si
3+xn
4-even with the ammonification metal mixed, accelerate the volatilization of solvent liquefied ammonia, obtain all mixing reactant.
3) by above-mentioned steps 2) all mixed reactant pack in crucible, advance synthetic furnace, and the through-flow speed high-purity N that is 200/min
2, keeping the stove internal gas pressure is normal pressure, with 5 ℃/min, is warmed up to 1200 ℃, insulation 6h, obtain synthetic product.
4) by above-mentioned steps 3) product after processing cools to 800 ℃ with 10 ℃/min, cuts off and adds thermoelectricity, continues to fill nitrogen, and furnace cooling, to normal temperature, takes out synthetic product, carries out product morphology observation and luminescent properties and tests.
Claims (3)
1. the synthetic method of a spherical silica-based nitrogen compound fluorescent material, is characterized in that, the step of the method is as follows:
1) ammonification of alkaline-earth metal and rare earth metal is dissolved:
Mole ratio according to each component of silica-based nitride, in mixing equipment, under normal temperature, high pure nitrogen condition, put into 0.02mol alkaline-earth metal and rare earth metal in the container cleaned up, the alkaline-earth metal that its mole number ratio is 199:1 ~ 4:1 and rare earth metal are dissolved in the dry liquefied ammonia solvent of 100ml ~ 200ml, stirring makes dissolving metal, forms solution ammonification metal, stand-by;
2) the ammonification metal is with spherical amorphous Si
3+xn
4-xevenly mix:
Take the spherical amorphous Si of activity of 1.4g by the component mole number ratio of silica-based nitride
3+xn
4-xpowder, by above-mentioned steps 1) in 100ml ~ 200ml solution ammonification metal be added to active spherical amorphous Si
3+xn
4-xin powder, stir the solvent liquefied ammonia volatilization made in solution ammonification metal, the ammonification metal is with M (NH
3)
xthe form supersaturation separate out, and be adsorbed on spherical amorphous Si
3+xn
4-xpowder surface, form intergranular precipitation at the spherical amorphous Si of activity
3+xn
4-xon powder, realize evenly mixing, obtain all mixed reactants of design requirements;
3) by above-mentioned steps 2) all mixed reactant pack in the synthetic furnace of nitrogen purging, the high-purity N that through-flow speed is 150-200ml/min
2, keeping the stove internal gas pressure is normal pressure, with 5 ℃/min, is warmed up to 1200-1380 ℃, insulation 4-10 hour, obtain synthetic product;
4) by above-mentioned steps 3) product after processing cools to 800 ℃ with 10 ℃/min, cuts off and adds thermoelectricity, continues to fill nitrogen and makes in stove to keep 0.1Mpa pressure, and furnace cooling, to normal temperature, stops filling nitrogen, the taking-up synthetic product.
2. the synthetic method of a kind of spherical silica-based nitrogen compound fluorescent material according to claim 1, it is characterized in that: described mixing equipment is the atmosphere protection glove box; Described synthetic furnace is the graphite heating synthesis device.
3. the synthetic method of a kind of spherical silica-based nitrogen compound fluorescent material according to claim 1, is characterized in that: the high-purity N that described nitrogen source of the gas is 99.99%
2; Described liquefied ammonia solvent is purity 99,99%, through the CaO drying treatment liquefied ammonia that dewaters.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103865534A (en) * | 2014-03-27 | 2014-06-18 | 浙江理工大学 | Preparation method of fluorescent nitride film material |
| CN105969332A (en) * | 2016-05-16 | 2016-09-28 | 浙江理工大学 | Synthesis method for coating M2Si5N8: Eu<2+> luminescent material with boron nitride |
| CN112973748A (en) * | 2021-02-22 | 2021-06-18 | 大连理工大学 | Synthesis method for in-situ preparation of propylene dimerization catalyst by taking ammonia as solvent |
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| CN103865534B (en) * | 2014-03-27 | 2015-09-02 | 浙江理工大学 | A kind of preparation method of nitride fluorescent thin-film material |
| CN105969332A (en) * | 2016-05-16 | 2016-09-28 | 浙江理工大学 | Synthesis method for coating M2Si5N8: Eu<2+> luminescent material with boron nitride |
| CN112973748A (en) * | 2021-02-22 | 2021-06-18 | 大连理工大学 | Synthesis method for in-situ preparation of propylene dimerization catalyst by taking ammonia as solvent |
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Application publication date: 20130626 |