CN104087290B - A kind of preparation method of nitride red fluorescent powder - Google Patents
A kind of preparation method of nitride red fluorescent powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 26
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002994 raw material Substances 0.000 claims description 22
- 239000000047 product Substances 0.000 claims description 17
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 15
- 229910052582 BN Inorganic materials 0.000 claims description 14
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000000643 oven drying Methods 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 239000006227 byproduct Substances 0.000 claims description 6
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims description 4
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 2
- 239000011575 calcium Substances 0.000 abstract description 23
- 229910052799 carbon Inorganic materials 0.000 abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052693 Europium Inorganic materials 0.000 abstract description 3
- 239000000428 dust Substances 0.000 abstract description 3
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical group [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052712 strontium Inorganic materials 0.000 abstract description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical group [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 229910052791 calcium Inorganic materials 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract description 2
- 238000011017 operating method Methods 0.000 abstract description 2
- 239000006184 cosolvent Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- MBEGFNBBAVRKLK-UHFFFAOYSA-N sodium;iminomethylideneazanide Chemical compound [Na+].[NH-]C#N MBEGFNBBAVRKLK-UHFFFAOYSA-N 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 208000013840 Non-involuting congenital hemangioma Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 1
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- Luminescent Compositions (AREA)
Abstract
The invention discloses the preparation method of a kind of nitride red fluorescent powder, its chemical structural formula is: (Ca1‑x Sr1‑x )Si5N8:Eu2x , wherein Ca is calcium constituent, and Sr is strontium element, and Si is element silicon, and N is nitrogen element, and Eu is europium element, wherein 0.05≤x≤0.20.Equipment needed thereby of the present invention requires simple, it is not necessary to glove box operates, and does not use carbon dust to reduce simultaneously, in products therefrom, the residual of free from admixture carbon, simplifies operating procedure, it is easy to batch production, the advantages such as it is high that the target product of synthesis has luminous efficiency, stable chemical nature, carbon free from foreign meter.
Description
Technical field
The invention discloses one and be mainly used in LED warm white room lighting, LED street lamp, LED backlight of LCD
Deng illumination and the preparation method of the nitride red fluorescent powder of display.
Background technology
White light LEDs has the advantages such as low-voltage, low energy consumption, long-life compared with conventional illumination sources, therefore suffers from domestic
Outer increasing concern.The most mode of currently acquired white light LEDs is blue-light LED chip and the yttrium-aluminium-garnet activated with cerium
Yellow fluorescent powder (YAG:Ce) is compound thus produces white light, and as the important component part of LED, LED fluorescent powder is subject in recent years
People more and more pay close attention to, but to there is also luminous efficiency at present the highest for YAG yellow fluorescent powder, and owing to lacking redness
Light emitting elements causes the shortcomings such as color rendering index is low.Therefore, in order to obtain the LED white light of more high color rendering index (CRI), need to add redness
Fluorescent material.
Schnick W team and Hintze H T team have carried out extensive work in early days, successfully synthesize M2Si5N8Silica-based
Nitride also obtains 600-630nm transmitting red material by Eu doping, quickly obtains application in LED.And quilt
The companies such as OSRAM and NICH IA are the earliest for the making of warm white LED.M2Si5N8: the synthesis of Eu system material is extremely difficult,
In early days the work of Schnick W et al. uses active alkaline-earth metal simple substance nitridation formed active binary nitride then with
Activity two imido silicon synthesizes in 1700 DEG C of high temperature above and nitrogen.These methods relate to active reactant, and condition is severe
Quarter, link complexity, be unfavorable for industrial volume production and application request.For the ease of industrialized production, reduce energy consumption, reduce into
This, update, in order to meet large-scale industrial production from raw material to technique.Therefore, it can stable in the air depositing
, simultaneous reactions temperature is relatively low has become as preparation M2Si5N8: the developing direction of Eu.
Summary of the invention
It is an object of the invention to provide a kind of luminous efficiency good, brightness is high, and not carbon-containing impurities is nitride red glimmering
Light powder, it effectively excites between 300-350 nm, and emission wavelength is between 600-700 nm, it is possible to better meet white light
A kind of nitride red fluorescent powder (Ca that the application of LED requires1-xSr1-x)Si5N8:Eu2xPreparation method.
The present invention is to be achieved through the following technical solutions: the preparation method of a kind of nitride red fluorescent powder, prepares nitrogen
The reaction equation of compound red fluorescence powder is:
(1-x)CaCN2+(Sr1-xEu2x)CO3+5/3Si3N4→(Ca1-xSr1-xEu2x)SiN+CO↑+CO2↑ (1)
1/2(1-x)CaCN2+1/2(Sr1-xEu2x)CO3+1/3Si3N4→(Ca1-xEux)AlySiN3+1/2CO↑+1/2CO2↑ (2)
(Sr1-xEu2x)CO3+(Ca1-xSr1-xEu2x)SiN+2/3Si3N4+2(Ca1-xEux)AlySiN3
→2(Ca1-xSr1-xEu2x)Si5N8+2yAlN+CO↑+CO2↑ (3)
The chemical structural formula of described nitride red fluorescent powder is as follows: (Ca1-xSr1-x)Si5N8:Eu2x, wherein Ca is calcium unit
Element, Sr is strontium element, and Si is element silicon, and N is nitrogen element, and Eu is europium element, wherein 0.05≤x≤0.20；
The step of the preparation method of nitride red fluorescent powder is as follows:
A, with CaCN2, SrCO3, Eu2O3And Si3N4For raw material；
B, according to chemical structural formula composition and stoichiometric proportion weigh above-mentioned raw materials；
C, in above-mentioned sample, add cosolvent, above-mentioned raw materials is sufficiently mixed with cosolvent, the matter of cosolvent and raw material
Amount ratio is in the range of 0.1%-0.5%；
D, by the above-mentioned raw material mixed at high temperature solid-state kiln roasting；
Product after E, roasting is through ball milling, washing, obtain nitride red fluorescent powder after drying.
Further improvement of the present invention is: silicon nitride is amorphous amorphous particle, and particle size is 300-500 nm.
Further improvement of the present invention is: cosolvent is the fluoride of II valency rare earth element.
Further improvement of the present invention is: the atmosphere in high temperature solid-state stove is N2；Gas pressure is 0.1 Pa, flow velocity
50-100 mL/min。
Further improvement of the present invention is: raw material roasting in two steps: first step sintering temperature is 1000 DEG C-1200 DEG C,
Time is 2-3h；Second step sintering temperature is 1500 DEG C-1550 DEG C, and the time is 4-6 h, after focusing on reaction end gas
Discharge.
Further improvement of the present invention is: holding vessel during raw material roasting is Mo crucible.
Further improvement of the present invention is: the product obtained after roasting sieves after levigate, is washed out, described washing
Sequentially passing through pickling, then through washing, wherein acid is hydrochloric acid, nitric acid or phosphoric acid, the molar concentration of acid is 5%-15%.
The present invention compared with prior art has the advantage that
1, the wide material sources needed for synthesis target product, it is not necessary to carbon dust or H2Reduce, free from admixture carbon in target product
Residual；
2, synthesis target product equipment is simple, normal pressure N2Atmosphere, safety coefficient is high, operates without glove box simultaneously, it is to avoid
The operating process that glove box is complicated, improves efficiency.
Accompanying drawing illustrates:
Fig. 1 be embodiment 1 excite figure；
Fig. 2 is the emission spectrum figure of embodiment 1；
Fig. 3 is the XRD spectra of embodiment 1.
Detailed description of the invention:
In order to deepen the understanding of the present invention, below in conjunction with embodiment and accompanying drawing, the invention will be further described, should
Embodiment is only used for explaining the present invention, is not intended that limiting the scope of the present invention.
The reaction equation preparing nitride red fluorescent powder is:
(1-x)CaCN2+(Sr1-xEu2x)CO3+5/3Si3N4→(Ca1-xSr1-xEu2x)SiN+CO↑+CO2↑ (1)
1/2(1-x)CaCN2+1/2(Sr1-xEu2x)CO3+1/3Si3N4→(Ca1-xEux)AlySiN3+1/2CO↑+1/2CO2↑ (2)
(Sr1-xEu2x)CO3+(Ca1-xSr1-xEu2x)SiN+2/3Si3N4+2(Ca1-xEux)AlySiN3
→2(Ca1-xSr1-xEu2x)Si5N8+2yAlN+CO↑+CO2↑ (3)
The chemical structural formula of nitride red fluorescent powder is as follows: (Ca1-xSr1-x)Si5N8:Eu2x, wherein Ca is calcium constituent,
Sr is strontium element, and Si is element silicon, and N is nitrogen element, and Eu is europium element, wherein 0.05≤x≤0.20；
The step of the preparation method of nitride red fluorescent powder is as follows:
A, with CaCN2, SrCO3, Eu2O3And Si3N4For raw material；
B, according to chemical structural formula composition and stoichiometric proportion weigh above-mentioned raw materials；
C, in above-mentioned sample, add cosolvent, above-mentioned raw materials is sufficiently mixed with cosolvent, the matter of cosolvent and raw material
Amount ratio is in the range of 0.1%-0.5%；
D, by the above-mentioned raw material mixed at high temperature solid-state kiln roasting；
Product after E, roasting is through ball milling, washing, obtain nitride red fluorescent powder after drying.
Silicon nitride is amorphous amorphous particle, and particle size is 300-500 nm, and cosolvent is II valency rare earth element
Fluoride, the atmosphere in high temperature solid-state stove is N2；Gas pressure is 0.1 Pa, and flow velocity 50-100 mL/min, raw material roasts in two steps
Burn: first step sintering temperature is 1000 DEG C-1200 DEG C, and the time is 2-3h；Second step sintering temperature is 1500 DEG C-1550 DEG C, time
Between be 4-6 h, discharge after reaction end gas is focused on, holding vessel during raw material roasting is Mo crucible, after roasting
To product sieve after levigate, be washed out, described washing sequentially passes through pickling, then through washing, wherein acid is hydrochloric acid, nitre
Acid or phosphoric acid, the molar concentration of acid is 5%-15%.
Equipment needed thereby of the present invention requires simple, it is not necessary to glove box operates, and does not use carbon dust to reduce, products therefrom simultaneously
The residual of middle free from admixture carbon, simplifies operating procedure, it is easy to batch production；It is high that the target product of synthesis has luminous efficiency, changes
Learn stable in properties, the advantage such as carbon free from foreign meter.
Embodiment 1:
Weigh CaCN respectively2 2.400g, SrCO3 4.207g, Eu2O3 0.528g, Si3N47.000g, AlN 0.038g with
And CaF2 Above raw material is added ethanol wet mixing 6 hours in beaker by 0.024g, puts into oven drying 24 hours, crosses 120 mesh sieves
Rear mix homogeneously, loads in boron nitride crucible so that it is 1100 DEG C of roastings 10 hours in nitrogen atmosphere, after being taken out by product of roasting
Grind, put into boron nitride crucible after crossing 200 mesh sieves, put it into 1550 DEG C of roastings of nitrogen atmosphere 12 hours.Products therefrom grinds
Wash with 10% nitric acid after sieving, be then washed with deionized post-drying and obtain Ca0.95Sr0.95Si5N8:Eu0.1Nitride
Red fluorescence powder.
Embodiment 2:
Weigh CaCN respectively22.160g, SrCO33.986g, Eu2O31.056g, Si3N47.000g, AlN 0.035g and
CaF2Above raw material is added ethanol wet mixing 6 hours in beaker by 0.026g, puts into oven drying 24 hours, after crossing 120 mesh sieves
Mix homogeneously, loads in boron nitride crucible, puts it in nitrogen atmosphere 1510 DEG C of roastings 10 hours, after being taken out by product of roasting
Grind, put into boron nitride crucible after crossing 200 mesh sieves, put it into 1550 DEG C of roastings of nitrogen atmosphere 12 hours.Products therefrom grinds
Wash with 10% nitric acid after sieving, be then washed with deionized post-drying and obtain Ca0.9Sr0.9Si5N8:Eu0.2Nitride is red
Color fluorescent material.
Embodiment 3:
Weigh CaCN respectively22.040g, SrCO33.764g, Eu2O31.584g, Si3N47.000g, AlN 0.033g and
CaF2Above raw material is added ethanol wet mixing 6 hours in beaker by 0.028g, puts into oven drying 24 hours, after crossing 120 mesh sieves
Mix homogeneously, loads in boron nitride crucible, puts it in nitrogen atmosphere 1510 DEG C of roastings 10 hours, after being taken out by product of roasting
Grind, put into boron nitride crucible after crossing 200 mesh sieves, put it into 1550 DEG C of roastings of nitrogen atmosphere 12 hours.Products therefrom grinds
Wash with 10% nitric acid after sieving, be then washed with deionized post-drying and obtain Ca0.85Sr0.85Si5N8:Eu0.3Nitride
Red fluorescence powder.
Embodiment 4:
Weigh CaCN respectively21.920g, SrCO33.543g, Eu2O32.112g, Si3N47.000g, AlN 0.031g and
CaF2Above raw material is added ethanol wet mixing 6 hours in beaker by 0.033g, puts into oven drying 24 hours, after crossing 120 mesh sieves
Mix homogeneously, loads in boron nitride crucible, puts it in nitrogen atmosphere 1510 DEG C of roastings 10 hours, after being taken out by product of roasting
Grind, put into boron nitride crucible after crossing 200 mesh sieves, put it into 1550 DEG C of roastings of nitrogen atmosphere 12 hours.Products therefrom grinds
Wash with 10% nitric acid after sieving, be then washed with deionized post-drying and obtain Ca0.8Sr0.8Si5N8:Eu0.4Nitride is red
Color fluorescent material.
It is last that it is noted that obviously above-described embodiment is only for clearly demonstrating example of the present invention, and also
The non-restriction to embodiment.For those of ordinary skill in the field, can also do on the basis of the above description
Go out change or the variation of other multi-form.Here without also cannot all of embodiment be given exhaustive.And thus drawn
What Shen went out obviously changes or changes among still in protection scope of the present invention.
Claims (3)
1. the preparation method of a nitride red fluorescent powder, it is characterised in that: step is as follows: weigh CaCN respectively2 2.400g,
SrCO3 4.207g, Eu2O3 0.528g, Si3N47.000g, AlN 0.038g and CaF2 0.024g by above raw material at beaker
Middle addition ethanol wet mixing 6 hours, puts into oven drying 24 hours, crosses mix homogeneously after 120 mesh sieves, loads in boron nitride crucible,
Make its 1100 DEG C of roastings 10 hours in nitrogen atmosphere, grind after product of roasting is taken out, after crossing 200 mesh sieves, put into boron nitride
Crucible, puts it into 1550 DEG C of roastings of nitrogen atmosphere 12 hours, and products therefrom grinds after sieving and washs, so with 10% nitric acid
After be washed with deionized post-drying and obtain Ca0.95Sr0.95Si5N8:Eu0.1Nitride red fluorescent powder.
2. the preparation method of a nitride red fluorescent powder, it is characterised in that: step is as follows: weigh CaCN respectively22.160g,
SrCO33.986g, Eu2O31.056g, Si3N47.000g, AlN 0.035g and CaF20.026g by above raw material in beaker
Add ethanol wet mixing 6 hours, put into oven drying 24 hours, cross mix homogeneously after 120 mesh sieves, load in boron nitride crucible, will
It puts in nitrogen atmosphere 1510 DEG C of roastings 10 hours, grinds after being taken out by product of roasting, puts into boron nitride after crossing 200 mesh sieves
Crucible, puts it into 1550 DEG C of roastings of nitrogen atmosphere 12 hours, and products therefrom grinds after sieving and washs, so with 10% nitric acid
After be washed with deionized post-drying and obtain Ca0.9Sr0.9Si5N8:Eu0.2Nitride red fluorescent powder.
3. the preparation method of a nitride red fluorescent powder, it is characterised in that: step is as follows: weigh CaCN respectively22.040g,
SrCO33.764g, Eu2O31.584g, Si3N47.000g, AlN 0.033g and CaF20.028g by above raw material in beaker
Add ethanol wet mixing 6 hours, put into oven drying 24 hours, cross mix homogeneously after 120 mesh sieves, load in boron nitride crucible, will
It puts in nitrogen atmosphere 1510 DEG C of roastings 10 hours, grinds after being taken out by product of roasting, puts into boron nitride after crossing 200 mesh sieves
Crucible, puts it into 1550 DEG C of roastings of nitrogen atmosphere 12 hours, and products therefrom grinds after sieving and washs, so with 10% nitric acid
After be washed with deionized post-drying and obtain Ca0.85Sr0.85Si5N8:Eu0.3Nitride red fluorescent powder.
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