CN103756678A - Red light-emitting tungstate fluorescent powder and preparation method thereof - Google Patents
Red light-emitting tungstate fluorescent powder and preparation method thereof Download PDFInfo
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- CN103756678A CN103756678A CN201410003791.3A CN201410003791A CN103756678A CN 103756678 A CN103756678 A CN 103756678A CN 201410003791 A CN201410003791 A CN 201410003791A CN 103756678 A CN103756678 A CN 103756678A
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Abstract
The invention relates to tungstate-based red light-emitting fluorescent powder and a preparation method thereof and belongs to the technical field of luminescent materials. The chemical formula of the fluorescent powder is Na(1-y)Li(y0Y(1-x)Eu(x)(WO4)2, wherein X is more than 0 and less than 1; Y is more than 0 and less than 0.5. The fluorescent powder is prepared by a solid-phase synthesis method; the strength of red light emitted by the stimulation of laser with the wavelength of 380nm used by a commercial LED blue-light semiconductor chip is more than two times that of commercial red powder (Eu doped with Y2O3). The fluorescent powder is suitable for being used as red powder for a display and a white light LED and has very good application prospect in the white light LED formed by the stimulation of the blue-light semiconductor chip.
Description
Technical field
The present invention relates to a kind of tungstate fluorescent material glowing, this fluorescent material chemical formula is: Na
1-yli
yy
1-xeu
x(WO
4)
2, wherein x span is (0-1), y span is (0-0.5), belongs to luminescent material technical field.
Background technology
Purity of color height and the large fluorescent material of luminous intensity are illumination and the critical material that shows field.Current commercial red phosphor mainly contains two kinds, wherein mixes the Y of Eu
2o
2s poor chemical stability, the SO producing
2be unfavorable for human body and contaminate environment.Another kind of commercial red phosphor is the Y that mixes Eu
2o
3although, chemically stable and environmental protection, the high-purity Y using
2o
3expensive, lack economy.In addition, although compare with conventional incandescent, within 1997, start the more energy-conservation and environmental protection of business-like white light LEDs, be described as the green light source of 21 century, but its needed fluorescent material that can effectively be excited by purple light or blue-light semiconductor chip and produce ruddiness is still in the exploratory stage, thereby cause the white light LEDs of current commercial blue-light semiconductor chip and yellow fluorescent powder YAG: Ce composition owing to lacking the red part of visible ray, obviously depart from color balance.
In sum, fluorescent material novel, cheap and efficiently red-emitting both can also can meet the demand of emerging white light LEDs for traditional lighting and demonstration field, had good economic worth.
The luminescent material that the tungstate of take is in recent years matrix has become one of focus of domestic and international commercial luminescent material research and development and intellecture property application, is also one of advanced subject of domestic and international academic fundamental research simultaneously.NaY (the WO that wherein Eu adulterates
4)
2the existing academic documents report of artificial monocrystalline and powder, but due to the factor such as luminescent properties is undesirable, cannot replace business red phosphor, therefore only rest on phase of basic research, the meaning that lacks commerciality application, and up to now, take both at home and abroad the patent report of the fluorescent material that this tungstate is foundation development.
Summary of the invention
The object of this invention is to provide a kind of tungstate fluorescent material glowing and preparation method thereof.A kind of tungstate fluorescent material that glows of the present invention, is characterized in that: this fluorescent material chemical formula is: Na
1-yli
yy
1-xeu
x(WO
4)
2, x wherein, y is molar fraction, 0 < x < 1,0 < y < 0.5.
The glow preparation method of tungstate fluorescent material, is characterized in that having following preparation process and step:
A. by above-mentioned stoichiometric ratio, take each component raw material;
B. by above-mentioned raw materials, in agate mortar, fully ground and mixed is even, pack subsequently alumina crucible with cover (30x50mm) into and put into the Shanghai SX2-6-13 of Yi Feng electric furnace company limited type chamber type electric resistance furnace, speed with 5 ℃/min is raised to 1100 ℃ from room temperature, be incubated after naturally cooling to room temperature after 8 hours and obtain the product powder that outward appearance is white in color, be the tungstate fluorescent material that glows.
The characteristic and performance of fluorescent material of the present invention
Now the specific and performance of relevant fluorescent material of the present invention is described below:
Described red phosphor, its feature is to use different material that required Na, Li, Y, Eu, W and O element is provided, and uses chemical solid phase synthesis process preparation, and final chemical constitution and x and y value meet above formula Na
1-yli
yy
1-xeu
x(WO
4)
2, x wherein, y is molar fraction, 0 < x < 1,0 < y < 0.5.
Under the incident light that this fluorescent material is less than 535nm at wavelength excites, can obtain emitting red light, centre wavelength is at 614 ± 10nm.
This fluorescent material and NaY (WO
4)
2isomorphism, but Component units size and composition are different, so the X-ray powder diffraction spectrogram of characterizing compounds structure is with respect to NaY (WO
4)
2there is angular deflection (referring to accompanying drawing 1).
The new phosphors that the present invention obtains can arrive the bright-coloured ruddiness of stimulated emission within the scope of blue light wavelength in UV-light, at exciting light, is the emission wavelength of the commercial LED blue-light semiconductor of 380nm(chip) time, luminous intensity is the Y that business red phosphor is mixed Eu
2o
3twice more than, and emmission spectrum distributes unanimously with it, red light pure (referring to accompanying drawing 2), therefore belongs to a kind of fluorescent material efficiently glowing.
The red phosphor that the present invention obtains is in order to ensure luminescent properties, must limit forming concentration, requiring the concentration y value scope of Li is (0-0.5), and Eu is due to close with Y ionic radius, therefore variable range is larger, and x value scope is (0-1), and above-mentioned scope does not all comprise cut off value, such as the y value of Li can not be zero, the rest may be inferred for all the other.
Red phosphor physics and stable chemical nature that the present invention obtains, do not need special protective measures; Fusing point and decomposition point be more than 1000 ℃, can bear the baking of heat treatment process hundreds of in device fabrication degree Celsius; Resistance to mechanical mill, is convenient to obtain the powder of appropriate particle size; Can obtain by solid-phase synthesis, be convenient to utilize conventional fluorescent powder production equipment directly and produce in a large number, reduce scrap build cost.
The fluorescent material that the present invention obtains both can replace existing business red phosphor for traditional lighting and demonstration field, also can be used as the rouge and powder of assembling white light LEDs, was particularly useful for the white light LEDs that blue-light semiconductor chip excites composition.
Accompanying drawing explanation
Fig. 1 is Na
0.8li
0.2y
0.91eu
0.09(WO
4)
2with Yttrium Tungstate sodium (NaY (WO
4)
2) the X-ray powder diffraction spectrogram contrast of (ICDD PDF# 48-0886).
Fig. 2 is the blue-light excited lower Na of 380nm
0.75li
0.25y
0.91eu
0.09(WO
4)
2with Eu doping Y
2o
3the luminous intensity contrast of (commercial product).
Embodiment
The fluorescent material of gained of the present invention can obtain by solid phase synthesis technique, and specific embodiment is as follows.
Embodiment 1.
Na
0.8li
0.2y
0.91eu
0.09(WO
4)
2, i.e. x=0.09, the synthesis step of y=0.2 fluorescent material:
(1) by stoichiometric ratio, take respectively the Y of 0.506g
2o
3, 0.078g Eu
2o
3, 0.209g Na
2cO
3, 2.28g WO
3and the Li of 0.036g
2cO
3powder, wherein Y
2o
3and Eu
2o
3be 99.9%, and Na
2cO
3, WO
3and Li
2cO
3for analytical pure;
(2) by above-mentioned raw materials, in agate mortar, fully ground and mixed is even.Pack subsequently alumina crucible with cover (30x50mm) into and put into the Shanghai SX2-6-13 of Yi Feng electric furnace company limited type chamber type electric resistance furnace, speed with 5 ℃/min is raised to 1100 ℃ from room temperature, is incubated after naturally cooling to room temperature after 8 hours and obtains the product powder that outward appearance is white in color.
Na
0.7li
0.3y
0.91eu
0.09(WO
4)
2, i.e. x=0.09, the synthesis step of y=0.3 fluorescent material:
(1) by stoichiometric ratio, take respectively the Y of 0.506g
2o
3, 0.078g Eu
2o
3, 0.183g Na
2cO
3, 2.28g WO
3and the Li of 0.054g
2cO
3powder, wherein Y
2o
3and Eu
2o
3be 99.9%, and Na
2cO
3, WO
3and Li
2cO
3for analytical pure;
(2) by above-mentioned raw materials, in agate mortar, fully ground and mixed is even.Pack subsequently alumina crucible with cover (30x50mm) into and put into the Shanghai SX2-6-13 of Yi Feng electric furnace company limited type chamber type electric resistance furnace, speed with 5 ℃/min is raised to 1100 ℃ from room temperature, is incubated after naturally cooling to room temperature after 8 hours and obtains the product powder that outward appearance is white in color.
Claims (3)
1. the tungstate fluorescent material that glows, is characterized in that: this fluorescent material chemical formula is: Na
1-yli
yy
1-xeu
x(WO
4)
2, x wherein, y is molar fraction, 0 < x < 1,0 < y < 0.5.
2. the preparation method of a kind of tungstate fluorescent material that glows according to claim 1, is characterized in that having following preparation process and step:
A. by above-mentioned stoichiometric ratio, take each component raw material;
B. by above-mentioned raw materials, in agate mortar, fully ground and mixed is even, pack subsequently alumina crucible with cover (30x50mm) into and put into the Shanghai SX2-6-13 of Yi Feng electric furnace company limited type chamber type electric resistance furnace, speed with 5 ℃/min is raised to 1100 ℃ from room temperature, be incubated after naturally cooling to room temperature after 8 hours and obtain the product powder that outward appearance is white in color, be the tungstate fluorescent material that glows.
3. the preparation method of a kind of tungstate fluorescent material that glows as claimed in claim 2, is characterized in that, each described component raw material is that purity is more than or equal to 99.9% Y
2o
3and Eu
2o
3, and analytically pure Li
2cO
3, Na
2cO
3, WO
3.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410003791.3A CN103756678A (en) | 2013-11-15 | 2014-01-06 | Red light-emitting tungstate fluorescent powder and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310572192.9 | 2013-11-15 | ||
| CN201310572192 | 2013-11-15 | ||
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111864023A (en) * | 2020-06-04 | 2020-10-30 | 江苏大学 | Sodium yttrium tungstate film material and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103320128A (en) * | 2013-06-24 | 2013-09-25 | 上海大学 | Red light-emitting tungstate fluorescent powder |
-
2014
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103320128A (en) * | 2013-06-24 | 2013-09-25 | 上海大学 | Red light-emitting tungstate fluorescent powder |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111864023A (en) * | 2020-06-04 | 2020-10-30 | 江苏大学 | Sodium yttrium tungstate film material and preparation method and application thereof |
| CN111864023B (en) * | 2020-06-04 | 2021-07-20 | 江苏大学 | Sodium yttrium tungstate film material and preparation method and application thereof |
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Application publication date: 20140430 |