CN104073253B - A kind of preparation method of oxynitride blue-green fluorescent powder - Google Patents
A kind of preparation method of oxynitride blue-green fluorescent powder Download PDFInfo
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- CN104073253B CN104073253B CN201310098110.1A CN201310098110A CN104073253B CN 104073253 B CN104073253 B CN 104073253B CN 201310098110 A CN201310098110 A CN 201310098110A CN 104073253 B CN104073253 B CN 104073253B
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- blue
- fluorescent powder
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Abstract
The invention provides a kind of oxynitride blue-green fluorescent powder, its chemical formula is: Eu
3y/2mg
3x/2al
( 64+z ) / 3-x-yo
( 32-z )n
z, wherein: 0 x 5,0 y 5,0 z 7.Its preparation method is as follows: Al(NO
3)
3, Eu(NO
3)
3, Mg(NO
3)
2be dissolved in water with citric acid, stir, evaporate to dryness; The mixture of evaporate to dryness is placed in retort furnace, calcining half hour, obtains ultra-fine nano-powder; Gained powder is put into crucible, puts into carbon tube furnace, high-temperature calcination; Gained powder is ground, was both obtained blue-green fluorescent powder.The luminescence band of obtained fluorescent material is at indigo plant-green light band, and luminosity is high, has satisfactory stability simultaneously, and the preparation of this fluorescent material has the advantage that technique is simple, cheaper starting materials is easy to get, preparation cost is low.
Description
Technical field
The present invention relates to phosphor material powder field, particularly a kind of preparation method of oxynitride blue-green fluorescent powder.
Background technology
Day by day serious along with world energy sources crisis, emerging energy project and energy-conserving and environment-protective industry become the problem of world's common concern.The advantage that white light LEDs because its luminous efficiency is high, energy consumption is few, operating voltage is low, the time of response is short, long service life, small product size are little etc. is given prominence to, has impayable competitive power, shows huge marketable value in interior lighting.Single LED chip is the white light that impossible send continuous spectrum, thus the method obtaining white light is at present generally carry out by fluorescent material the monochromatic ray that conversion LED sends, and combination obtains the white light (as traditional blue light+bloom technology and burst of ultraviolel three primary colours technology etc.) needed for human eye.
Present stage, the implementation of main flow white light LEDs was that LED chip adds fluorescence transition material, and by blue light and gold-tinted, or the mutual compound of blue, green, red three primary colours produces white light.Such as, on ultraviolet LED, coating can by the blue powder BAM:Eu of ultraviolet excitation
2+, green powder BaSiO
4: Eu
2+, rouge and powder Y
2o
2s:Eu
3+, this implementation tool in color developing has great advantage, and colour rendering index can reach 96, but needs the allotment of three kinds of dissimilar fluorescent material, complex process, is difficult to keep homogeneity of product.This aluminate and silicate fluorescent powder, chemical stability, thermostability are all poor.Oxynitride pottery is as a class formation pottery, and O/N forms stable rigid backbone, has outstanding physics and chemistry stability.Rear-earth-doped oxynitride just attracts the extensive attention of whole world researchist with the luminescent properties of its excellence, physics and chemistry stability, it has very large advantage in color developing and thermostability, becomes the preferred material of high-grade place illumination gradually.
Aluminum oxynitride is as Al
2o
3with the sosoloid of AlN, be a class crystalline ceramics, have excellent optics, machinery, physics and chemistry stability, intensity is high, and hardness is large, is the high-temperature structural ceramics of a class excellence, is widely used in the fields such as laser, plate armour and infrared acquisition.Rare earth doping fluorescent powder aluminum oxynitride based on aluminum oxynitride matrix: Eu
2+have excellent physics, chemical stability and optical property, the band gap of aluminum oxynitride is at more than 5eV, and being with of rare earth luminous ion just can be present among matrix can be with, and when being subject to high-energy photons and exciting, sends blue green light.The mode that can apply bluish-green powder and rouge and powder on LED chip directly obtains white light.
Bluish-green powder has the wave band feature of blue light and green glow simultaneously, and emission wavelength has large halfwidth, thus combines with ruddiness, forms good color developing.
But traditional high-temperature solid phase reaction method prepares aluminum oxynitride: Eu
2+fluorescent material, condition is harsher, at high temperature 1800
omore than C, carries out long-time heat preservation, and having high input of equipment and the energy, cost is high.
Summary of the invention
The object of this invention is to provide a kind of blue-green fluorescent powder, preparation method thereof of low cost.Adopt citric acid method, to be easy to get with raw material, cheap nitrate, use Al(NO
3)
3, Eu(NO
3)
3, Mg(NO
3)
2with citric acid as starting raw material, high-level efficiency oxynitride blue-green fluorescent powder can be obtained at lesser temps isothermal treatment for short time.
The present invention is achieved through the following technical solutions:
Oxynitride blue-green fluorescent powder of the present invention, is characterized in that its chemical formula is: Eu
3y/2mg
3x/2al
(64+z)/3-x-yo
(32-z)n
z, wherein: 0 x 5,0 y 5,0 z 7.
The preparation method of oxynitride blue-green fluorescent powder of the present invention, step is as follows:
1. according to metering ratio, Al(NO
3)
3, Eu(NO
3)
3, Mg(NO
3)
2be dissolved in water with citric acid, in magnetic stirring apparatus, 60-100
ounder C, constant temperature stirs, and evaporate to dryness, obtains xerogel; Wherein the molar weight of citric acid is 0.5-2.5 times of whole cation mole number.
2. above-mentioned xerogel is placed in retort furnace, at 150-300
ocalcine half hour under C, obtain ultra-fine nano-powder.
3. gained powder is put into BN crucible, put into carbon tube furnace, at 1500-3000
ocalcine under C, insulation 1-3h, after insulation terminates, is ground gained powder, is namely obtained blue-green fluorescent powder.
the invention has the beneficial effects as follows:this project adopts rare earth ion doped aluminum oxynitride matrix, by citric acid method, utilizes cheap Al(NO
3)
3, Eu(NO
3)
3, citric acid as initial powder, decompose residual C during citric acid thermal treatment as reduction C source.Owing to not having expensive AlN in raw material, this method preparation cost comparatively solid reaction process reduces more than 60%, and the luminescence band of this fluorescent material is at indigo plant-green light band, and luminosity is high, has the stability of oxynitride excellence simultaneously.
Accompanying drawing explanation
Fig. 1 is the utilizing emitted light spectrogram of blue-green fluorescent powder under 365nm excites.
Embodiment
According to structural formula Eu
3y/2mg
3x/2al
(64+z)/3-x-yo
(32-z)n
z, 0 x 5,0 y 5,0 z 7, the powder Al(NO required for weighing
3)
3, Eu(NO
3)
3, Mg(NO
3)
2, the molar weight of required citric acid is 1.5 times of whole cation mole number.
All powders put into the aqueous solution, fully stirs, dissolve, in magnetic stirring apparatus, 80
ounder C, constant temperature stirs, and evaporate to dryness, obtains xerogel.
Above-mentioned gained xerogel is put into aluminum oxide porcelain boat, puts in retort furnace, 200
oc calcines half hour, obtains ultra-fine nano-powder.
Citric acid decomposes a large amount of C of generation, and gained powder is brown.Contain the mixture of nitrate and C in powder, utilize the starting powder that this liquid phase method synthesizes, particle diameter reaches nanometer scale, and element reaches the abundant mixing between atomic level, and the sintering activity of powder is high especially.Therefore, solid state reaction can be carried out under low temperature again and obtain target product.
Gained superfine powder is put into BN crucible, puts into carbon tube furnace, using the C of combustion residue as reductive agent, in temperature 1650
obe incubated 2h under C, wait body of heater naturally cooling, block powder can be obtained.
Gained powder is put into mortar, is ground 10 minutes, both obtained blue-green fluorescent powder.The utilizing emitted light spectrogram of the fluorescent material that the present embodiment obtains under 365nm excites as shown in Figure 1.
Claims (4)
1. a preparation method for oxynitride blue-green fluorescent powder, is characterized in that: Al(NO
3)
3, Eu(NO
3)
3, Mg(NO
3)
2be dissolved in water with citric acid, stir, evaporate to dryness; The mixture of evaporate to dryness is placed in retort furnace, calcining half hour, obtains ultra-fine nano-powder; Gained powder is put into crucible, puts into carbon tube furnace, high-temperature calcination; Gained powder is ground, is namely obtained blue-green fluorescent powder; Described Al(NO
3)
3, Eu(NO
3)
3, Mg(NO
3)
2by chemical formula Eu
3y/2mg
3x/2al
(64+z)/3-x-yo
(32-z)n
z, wherein: the metering of 0 x 5,0 y 5,0 z 7 is than mixing, and the molar weight of citric acid is above-mentioned whole cationic 0.5-1.5 times.
2. the preparation method of oxynitride blue-green fluorescent powder according to claim 1, is characterized in that: Al(NO
3)
3, Eu(NO
3)
3, Mg(NO
3)
2be 60-100 with the temperature of citric acid mixed dissolution
oc.
3. the preparation method of oxynitride blue-green fluorescent powder according to claim 1, is characterized in that: the calcining temperature in retort furnace is 150-300
oc.
4. the preparation method of oxynitride blue-green fluorescent powder according to claim 1, is characterized in that: in carbon tube furnace, temperature is 1500-2000
oc.
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|---|---|---|---|
| CN201310098110.1A CN104073253B (en) | 2013-03-26 | 2013-03-26 | A kind of preparation method of oxynitride blue-green fluorescent powder |
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| CN104073253B true CN104073253B (en) | 2016-04-27 |
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| CN101629077A (en) * | 2009-08-14 | 2010-01-20 | 上海芯光科技有限公司 | Multi-component oxynitride or nitride base fluorescent powder and preparation method thereof |
| KR101471449B1 (en) * | 2011-09-08 | 2014-12-10 | 피에스아이 주식회사 | micro size phosphor for minimizing scattering |
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