CN104650861A - Simple method for preparing alkali-earth nitride red fluorescent powder - Google Patents
Simple method for preparing alkali-earth nitride red fluorescent powder Download PDFInfo
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- CN104650861A CN104650861A CN201510073264.4A CN201510073264A CN104650861A CN 104650861 A CN104650861 A CN 104650861A CN 201510073264 A CN201510073264 A CN 201510073264A CN 104650861 A CN104650861 A CN 104650861A
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- alkaline earth
- red fluorescence
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- nitride
- fluorescence powder
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Abstract
The invention provides a simple method for preparing alkali-earth nitride Ca1-x-ySrxAlSiN3:yEu<2+> (wherein x is smaller than 1 and greater than or equal to 0, and y is smaller than or equal to 0.30 and greater than 0) red fluorescent powder. The method comprises the following main preparation processes: mixing alkali-earth carbonate, europium oxide, nitrides or oxides of silicon and aluminum and a little of a fluxing agent evenly in air, pressing into a bulk material, and then putting into a molybdenum boat with carbon dust; carrying out heat preservation in high-purity nitrogen, cooling and removing surface carbon dust; and crushing a sample, washing and sieving to obtain a finished product. The alkali-earth nitride red fluorescent powder provided by the invention has the characteristics that raw materials with stable properties are adopted; a glove box is not needed to operate; the preparation technology is simple; the synthetic temperature is relatively low; the alkali-earth nitride red fluorescent powder can be prepared at ordinary pressure; and the prepared nitride fluorescent powder is high in purity, not easy to pollute, uniform in particle size, good in stability, high in luminous efficiency and excellent in performance.
Description
Technical field
The invention belongs to rare earth luminescent material field, be specifically related to a kind of simple and easy method preparing alkaline earth nitride red fluorescence powder, this fluorescent material can be used for solid state LED and low pressure mercury lamp illumination, backlight and plant growth lamp field.
Background technology
Along with developing rapidly of LED industry, the requirement of solid-state illumination field to white light is also more and more higher, require the light efficiency of white LED lamp and color developing more and more higher.The YAG fluorescent powder of industrial scale production lacks the composition of ruddiness, and after becoming lamp, colour rendering index is not high, often needs the red fluorescence powder by adding long-wave band to improve its colour rendering index, thus obtains low color temperature white light LED product.The fluorescent material of long-wave band mainly divides sulfide in the market, nitride, silicate three class.Sulfide red fluorescent material pollutes comparatively large, can produce very strong stink, and perishable support, be now eliminated gradually.And silicate orange red fluorescence powder alkalescence is strong, chemistry and physical properties also stable not.Nitride red fluorescent powder stability is very excellent, becomes main product gradually, but its manufacturing cost is high, is difficult to widespread use.
Up to the present, in industrial production, nitride mainly adopts high temperature solid-state method, raw materials used is alkaline earth nitride, character is unstable, needs to operate after exclusion of water, oxygen in glove box, and generally will at about 1800 DEG C high temperature, synthesize under 10 MPa left and right high pressure, high to the requirement of equipment, energy consumption and cost are all very high, and operational danger is larger.As Mitsubishi Chemical uses the corresponding metal in molecular formula to carry out nitrogenize as initial reactant in United States Patent (USP), then synthesize such twinkler at high temperature under high pressure, this invention thinks that this method of selection can prepare high-quality Nitride phosphor.BaCO is utilized in US Patent No. 7671529
3, SrCO
3, Eu
2o
3, carbon dust, Si
3n
4for Material synthesis (Ba
1-xsr
x)
2-y-0.5zsi
5n
8-zo
z: Eu
2+nitride red fluorescent powder, although this method avoids the operation of glove box, nitride is obtained by adding carbon reducing agent, but this method has a unavoidable problem in actual production: have more residual carbon dust in product, have a strong impact on the optical property of fluorescent material, and temperature of reaction is also higher, energy consumption is high.
Summary of the invention
The present invention, for solving the problems of the technologies described above, prepares the method for high purity alkaline earth nitride red fluorescent powder under providing a kind of normal pressure of simple and easy, handled easily.
The present invention is the technical scheme solving the problems of the technologies described above employing:
A preparation method for alkaline earth nitride red fluorescence powder, is characterized in that, comprises the following steps:
(1) take reaction raw materials and mix, being raw materials usedly
(a). alkaline earth carbonate,
(b). europium sesquioxide,
(c). the nitride of silicon or oxide compound, the nitride of aluminium or oxide compound, and
(d). a small amount of fusing assistant;
(2) mixture is loaded in mould, compression moulding;
(3) compression moulding thing is placed on is equipped with in the molybdenum boat of carbon dust, react in nitrogen atmosphere;
(4), after cooling, remove surperficial carbon dust, wash after sample broke, sieve, get product.
A preparation method for above-mentioned alkaline earth nitride red fluorescence powder, is characterized in that, comprise the following steps:
(1) by chemical formula Ca
1-x-ysr
xalSiN
3: yEu
2+in the stoichiometric ratio of each element take reaction raw materials, add fusing assistant, mix;
(2) mixture is loaded in mould, compression moulding;
(3) forming composition is placed on is equipped with in the molybdenum boat of carbon dust, react in nitrogen atmosphere;
(4) cooling after reaction, removes surperficial carbon dust, washs after sample broke, sieve, get product.
Preferably, in step (1), chemical formula is Ca
1-x-ysr
xalSiN
3: yEu
2+, wherein, 0≤x < 1.0,0 < y≤0.30.
Preferred further, step (1) reaction raw materials used is
(a). alkaline earth Strontium carbonate powder, calcium carbonate,
(b). europium sesquioxide,
(c). silicon-dioxide or silicon nitride, aluminium nitride or aluminum oxide,
Above-mentioned substance purity is all more than analytical pure.
Preferably, the fusing assistant in step (1) is BaF
2, CaF
2, H
3bO
3and MgF
2in one or more, and the amount added is 0.5% ~ 10% of reaction raw materials total mass.
Preferably, loaded by mixture in mould and use pressing machine compression moulding under 2-50 ton pressure, the thickness of forming composition is 2-50 millimeter.
Preferably, in nitrogen atmosphere, temperature of reaction is 1300-1600 DEG C, normal pressure, insulation 2-8 hour.
Preferably, nitrogen is high pure nitrogen, and purity is more than 99.9%.
A kind of alkaline earth nitride red fluorescence powder, its chemical constitution is: Ca
1-x-ysr
xalSiN
3: yEu
2+, wherein, 0≤x < 1.0,0 < y≤0.30.
Preferably, the element in chemical formula derives from Strontium carbonate powder, calcium carbonate respectively, europium sesquioxide, and the source of silicon is silicon-dioxide or silicon nitride, and the source of aluminium is aluminium nitride or aluminum oxide, and purity is all more than analytical pure.
Beneficial effect of the present invention:
Feature of the present invention is that character of use is stablized, the raw material of price cheapness, in atmosphere can stable existence, and do not need to operate under the severe condition of anhydrous and oxygen-free, preparation technology is simple.After reaction raw materials pressure being formed block by high pressure, molecule distance between reaction raw materials is reduced, temperature of reaction reduces, as long as and prepare at ambient pressure, overcome the restriction usually needing in traditional method to synthesize under elevated pressure conditions, thus significantly reduce the danger of production cost and operation, simplify preparation technology, and the Nitride phosphor purity prepared is high, owing to being blocks, can not be inner by Carbon dust pollution, only surface carbon need be wiped off, fluorescent material uniform particle sizes, good stability, luminous efficiency is high, excellent performance, high to blue light region 250-550nm launching efficiency in ultraviolet, launch main peak scope and can cover 590-690nm, be applicable to low pressure mercury lamp (launching the ultraviolet being positioned at 253.7nm based on peak position), near-ultraviolet light (380-410nm) and blue light (430-470nm) are as excitation light source, be applied in luminescent lamp, the illumination of LED, backlight and plant growth lamp field.
Accompanying drawing explanation
Fig. 1 is the excitation-emission spectrogram of the embodiment of the present invention 1;
Fig. 2 is the excitation-emission spectrogram of the embodiment of the present invention 2;
Fig. 3 is the excitation-emission spectrogram of the embodiment of the present invention 3;
Fig. 4 is the excitation-emission spectrogram of the embodiment of the present invention 4;
Fig. 5 is the scanning electron microscope (SEM) photograph (SEM) of the embodiment of the present invention 4.
Embodiment
Embodiment 1
Alkaline earth nitride red fluorescence powder Ca
0.072sr
0.92alSiN
3: 0.008Eu
2+the preparation of (x=0.92, y=0.008), stoichiometrically takes raw material:
SrCO
3:2.716g
CaCO
3:0.144g
AlN:0.820g
Si
3N
4:0.935g
Eu
2O
3:0.0282g
BaF
2:0.093g
After institute's raw materials weighing is mixed, load in mould and use pressing machine compression moulding under 30 tons of pressure, thickness is 20 millimeters, is then placed in carbon dust, be incubated 8 hours in 1350 DEG C in nitrogen atmosphere after, cool, remove surperficial carbon dust and can nitride red fluorescent powder be obtained after fragmentation.
Embodiment 2
Alkaline earth nitride red fluorescence powder Ca
0.15sr
0.80alSiN
3: 0.05Eu
2+the preparation of (x=0.80, y=0.05), stoichiometrically takes raw material:
SrCO
3:2.362g
CaCO
3:0.300g
AlN:0.820g
Si
3N
4:0.935g
Eu
2O
3:0.176g
MgF
2:0.119g
After institute's raw materials weighing is mixed, load in mould and use pressing machine compression moulding under 50 tons of pressure, thickness is 50 millimeters, is then placed in carbon dust, be incubated 7 hours in 1400 DEG C in nitrogen atmosphere after, cool, remove surperficial carbon dust and can nitride red fluorescent powder be obtained after fragmentation.
Embodiment 3
Alkaline earth nitride red fluorescence powder Ca
0.20sr
0.65alSiN
3: 0.15Eu
2+the preparation of (x=0.65, y=0.15), stoichiometrically takes raw material:
SrCO
3:1.920g
CaCO
3:0.400
AlN:0.820g
SiO
2:1.202g
Eu
2O
3:0.528g
CaF
2:0.0487g
After institute's raw materials weighing is mixed, load in mould and use pressing machine compression moulding under 10 tons of pressure, thickness is 2 millimeters, is then placed in carbon dust, be incubated 3 hours in 1600 DEG C in nitrogen atmosphere after, cool, remove surperficial carbon dust and can nitride red fluorescent powder be obtained after fragmentation.
Embodiment 4
Alkaline earth nitride red fluorescence powder Ca
0.99alSiN
3: 0.01Eu
2+the preparation of (x=0, y=0.01), stoichiometrically takes raw material:
CaCO
3:1.980g
AlN:0.820g
Si
3N
4:0.935g
Eu
2O
3:0.0352g
CaF
2:0.095g
After institute's raw materials weighing is mixed, load in mould and use pressing machine compression moulding under 2 tons of pressure, thickness is 30 millimeters, is then placed in carbon dust, be incubated 4 hours in 1450 DEG C in nitrogen atmosphere after, cool, remove surperficial carbon dust and can nitride red fluorescent powder be obtained after fragmentation.
Table 1 is the optical parametric of embodiment 1-4.
The optical parametric of table 1 embodiment 1-4
Embodiment 5
Alkaline earth nitride red fluorescence powder Ca
0.999alSiN
3: 0.001Eu
2+the preparation of (x=0, y=0.001), stoichiometrically takes raw material:
CaCO
3:1.998g
Al
2O
3:1.020g
SiO
2:1.202g
Eu
2O
3:0.00352g
H
3BO
3:0.148g
After institute's raw materials weighing is mixed, load in mould and use pressing machine compression moulding under 40 tons of pressure, thickness is 40 millimeters, is then placed in carbon dust, be incubated 6 hours in 1300 DEG C in nitrogen atmosphere after, cool, remove surperficial carbon dust and can nitride red fluorescent powder be obtained after fragmentation.
Embodiment 6
Alkaline earth nitride red fluorescence powder Ca
0.30sr
0.40alSiN
3: 0.30Eu
2+the preparation of (x=0.40, y=0.30), stoichiometrically takes raw material:
SrCO
3:1.181g
CaCO
3:0.600g
AlN:0.820g
Si
3N
4:0.935g
Eu
2O
3:1.056g
BaF
2:0.306g
After institute's raw materials weighing is mixed, load in mould and use pressing machine compression moulding under 25 tons of pressure, thickness is 10 millimeters, is then placed in carbon dust, be incubated 8 hours in 1300 DEG C in nitrogen atmosphere after, after cooling fragmentation, nitride red fluorescent powder can be obtained.
Embodiment 7
Alkaline earth nitride red fluorescence powder Ca
0.60sr
0.20alSiN
3: 0.20Eu
2+the preparation of (x=0.20, y=0.20), stoichiometrically takes raw material:
SrCO
3:0.591g
CaCO
3:1.200g
AlN:0.820g
SiO
2:1.202g
Eu
2O
3:0.704g
H
3BO
3:0.145g
After institute's raw materials weighing is mixed, load in mould and use pressing machine compression moulding under 10 tons of pressure, thickness is 25 millimeters, is then placed in carbon dust, be incubated 5 hours in 1450 DEG C in nitrogen atmosphere after, cool, remove surperficial carbon dust and can nitride red fluorescent powder be obtained after fragmentation.
Embodiment 8
Alkaline earth nitride red fluorescence powder Ca
0.88sr
0.10alSiN
3: 0.02Eu
2+the preparation of (x=0.10, y=0.02), stoichiometrically takes raw material:
SrCO
3:0.295g
CaCO
3:1.760g
Al
2O
3:1.020g
Si
3N
4:0.935g
Eu
2O
3:0.0704g
H
3BO
3:0.198g
After institute's raw materials weighing is mixed, load in mould and use pressing machine compression moulding under 15 tons of pressure, thickness is 15 millimeters, is then placed in carbon dust, be incubated 3 hours in 1500 DEG C in nitrogen atmosphere after, cool, remove surperficial carbon dust and can nitride red fluorescent powder be obtained after fragmentation.
Embodiment 9
Alkaline earth nitride red fluorescence powder Ca
0.49sr
0.50alSiN
3: 0.01Eu
2+the preparation of (x=0.5, y=0.01), stoichiometrically takes raw material:
SrCO
3:1.476g
CaCO
3:0.980g
AlN:0.820g
Si
3N
4:0.935g
Eu
2O
3:0.0352g
CaF
2:0.075g
After institute's raw materials weighing is mixed, load in mould and use pressing machine compression moulding under 35 tons of pressure, thickness is 10 millimeters, is then placed in carbon dust, be incubated 5 hours in 1600 DEG C in nitrogen atmosphere after, cool, remove surperficial carbon dust and can nitride red fluorescent powder be obtained after fragmentation.
Embodiment 10
Alkaline earth nitride red fluorescence powder Ca
0.50sr
0.42alSiN
3: 0.08Eu
2+the preparation of (x=0.42, y=0.08), stoichiometrically takes raw material:
SrCO
3:1.240g
CaCO
3:1.000g
Al
2O
3:1.020g
SiO
2:1.202g
Eu
2O
3:0.282g
CaF
2:0.228g
After institute's raw materials weighing is mixed, load in mould and use pressing machine compression moulding under 18 tons of pressure, thickness is 20 millimeters, is then placed in carbon dust, be incubated 2 hours in 1600 DEG C in nitrogen atmosphere after, after cooling fragmentation, nitride red fluorescent powder can be obtained.
Claims (10)
1. a preparation method for alkaline earth nitride red fluorescence powder, is characterized in that, comprises the following steps:
(1) take reaction raw materials and mix, being raw materials usedly
(a). alkaline earth carbonate,
(b). europium sesquioxide,
(c). the nitride of silicon or oxide compound, the nitride of aluminium or oxide compound, and
(d). a small amount of fusing assistant;
(2) mixture is loaded in mould, compression moulding;
(3) compression moulding thing is placed on is equipped with in the molybdenum boat of carbon dust, react in nitrogen atmosphere;
(4), after cooling, remove surperficial carbon dust, wash after sample broke, sieve, get product.
2. a preparation method for alkaline earth nitride red fluorescence powder as claimed in claim 1, is characterized in that, comprise the following steps:
(1) by chemical formula Ca
1-x-ysr
xalSiN
3: yEu
2+in the stoichiometric ratio of each element take reaction raw materials, add fusing assistant, mix;
(2) mixture is loaded in mould, compression moulding;
(3) forming composition is placed on is equipped with in the molybdenum boat of carbon dust, react in nitrogen atmosphere;
(4) cooling after reaction, removes surperficial carbon dust, washs after sample broke, sieve, get product.
3. the preparation method of alkaline earth nitride red fluorescence powder as claimed in claim 2, is characterized in that, in step (1), chemical formula is Ca
1-x-ysr
xalSiN
3: yEu
2+, wherein, 0≤x < 1.0,0 < y≤0.30.
4. the preparation method of alkaline earth nitride red fluorescence powder as claimed in claim 1 or 2, it is characterized in that, step (1) reaction raw materials used is
(a). alkaline earth Strontium carbonate powder, calcium carbonate,
(b). europium sesquioxide,
(c). silicon-dioxide or silicon nitride, aluminium nitride or aluminum oxide,
Above-mentioned substance purity is all more than analytical pure.
5. the preparation method of alkaline earth nitride red fluorescence powder as claimed in claim 1 or 2, it is characterized in that, the fusing assistant in step (1) is BaF
2, CaF
2, H
3bO
3and MgF
2in one or more, and the amount added is 0.5% ~ 10% of reaction raw materials total mass.
6. the preparation method of alkaline earth nitride red fluorescence powder as claimed in claim 1 or 2, it is characterized in that, loaded by mixture in mould and use pressing machine compression moulding under 2-50 ton pressure, the thickness of forming composition is 2-50 millimeter.
7. the preparation method of alkaline earth nitride red fluorescence powder as claimed in claim 1 or 2, it is characterized in that, in nitrogen atmosphere, temperature of reaction is 1300-1600 DEG C, normal pressure, insulation 2-8 hour.
8. the preparation method of alkaline earth nitride red fluorescence powder as claimed in claim 1 or 2, it is characterized in that, nitrogen is high pure nitrogen, and purity is more than 99.9%.
9. an alkaline earth nitride red fluorescence powder, is characterized in that, its chemical constitution is: Ca
1-x-ysr
xalSiN
3: yEu
2+, wherein, 0≤x < 1.0,0 < y≤0.30.
10. alkaline earth nitride red fluorescence powder as claimed in claim 9, it is characterized in that, the element in chemical formula derives from Strontium carbonate powder, calcium carbonate respectively, europium sesquioxide, the source of silicon is silicon-dioxide or silicon nitride, and the source of aluminium is aluminium nitride or aluminum oxide, and purity is all more than analytical pure.
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| CN101974332A (en) * | 2010-09-15 | 2011-02-16 | 北京科技大学 | Oxide fluorescent material and preparation method thereof |
| CN103820107A (en) * | 2014-03-24 | 2014-05-28 | 中国科学院上海硅酸盐研究所 | Method for removing carbon powder from fluorescent powder prepared by carbothermal reduction reaction |
| CN104087294A (en) * | 2014-07-28 | 2014-10-08 | 江苏罗化新材料有限公司 | Carbon reduction preparation method of red nitride phosphor |
-
2015
- 2015-02-10 CN CN201510073264.4A patent/CN104650861B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2022836A1 (en) * | 2004-08-27 | 2009-02-11 | DOWA Electronics Materials Co., Ltd. | Phosphor and manufacturing method for the same, and light source using the same |
| CN101974332A (en) * | 2010-09-15 | 2011-02-16 | 北京科技大学 | Oxide fluorescent material and preparation method thereof |
| CN103820107A (en) * | 2014-03-24 | 2014-05-28 | 中国科学院上海硅酸盐研究所 | Method for removing carbon powder from fluorescent powder prepared by carbothermal reduction reaction |
| CN104087294A (en) * | 2014-07-28 | 2014-10-08 | 江苏罗化新材料有限公司 | Carbon reduction preparation method of red nitride phosphor |
Non-Patent Citations (2)
| Title |
|---|
| 吕建军: "白光LED用CaAlSiN3：Eu2+荧光粉的制备及性能研究", 《中国优秀硕士学位论文全文数据库（基础科学辑）》 * |
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Effective date of registration: 20170615 Address after: 226200 Nantong City, Qidong Province Economic Development Zone, No. triumph Road, No. 1 Patentee after: Qidong Green Green Engineering Co., Ltd. Address before: Guangdong city of Jiangmen province Tangxia 529030 factory town Pengjiang District Xinchang Wonsan Aberdeen Industrial Zone Patentee before: Yuanda Phosphors Co., Ltd. |