CN102604633A - Tetratungstate red phosphor powder and preparation method thereof - Google Patents
Tetratungstate red phosphor powder and preparation method thereof Download PDFInfo
- Publication number
- CN102604633A CN102604633A CN2012100283073A CN201210028307A CN102604633A CN 102604633 A CN102604633 A CN 102604633A CN 2012100283073 A CN2012100283073 A CN 2012100283073A CN 201210028307 A CN201210028307 A CN 201210028307A CN 102604633 A CN102604633 A CN 102604633A
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- red phosphor
- phosphor powder
- fluorescent material
- tungstate
- europium
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- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
The invention provides a tetratungstate red phosphor powder and a preparation method thereof. The tetratungstate red phosphor powder treats tungstate as a matrix and has a chemical formula of Na5La1-xEux(WO4)4, wherein the doped concentration of europium ions is equal to or greater than 0.1 and equal to or less than 1.0. The red phosphor powder of the invention can be excited by near-ultraviolet light and blue LED (light emitting diode) chips and has the characteristics of good luminescent performance and good chemical stability, the luminescent performance of the red phosphor powder can be further enhanced through changing the doped rare earth, and the red phosphor powder which has the advantages of simple preparation technology and low production cost is an excellent red phosphor powder for a high color rendering white LED.
Description
Technical field
The present invention relates to rare earth luminescent material and solid-state illumination technical field, especially relate to a kind of four tungstate red fluorescent powders and preparation method thereof.
Background technology
White light LEDs is as a kind of novel environmental type solid light source, has that WV is low, low in energy consumption, safety is high, a series of advantages such as long service life, environmental friendliness and high energy efficiency, is the developing direction of following lighting source.In led light source, the performance of fluorescent material has determined the technical indicators such as luminous efficiency, colour rendering index, colour temperature and work-ing life of LED, and therefore, fluorescent material has critical role in white light LEDs, receives extensive concern.
At present, realize that the method for white light LEDs mainly contains three kinds: first kind is many chip methods, with the led chip of three kinds of colors of red, green, blue, utilizes the three primary colors principle to send white light according to certain ratio combination.Second kind is integrated single-chip method, also claims the multiple quantum well method, promptly in a chip, utilizes a plurality of active coatings to make led chip directly send white light.The third is the fluorescent material transformation approach, on near-ultraviolet light or blue-light LED chip, applies fluorescent material, and white light, the blue-light excited YAG:Ce that wherein adopts the InGaN chip to be launched are sent in the light mixing that light that chip sends and chip excitated fluorescent powder send
3+Fluorescent material realizes that the white light LEDs technical development is rapid, has realized the commercialization utilization.The third method is that utilization at most also is the most sophisticated at present, but shortcoming is also fairly obvious, owing to be that blue light and gold-tinted two primary colours are compounded to form white light, lacks red light portion in its composition, makes colour rendering index on the low side.In near ultraviolet excitation red, green, blue three primary colors fluorescent powder method, mainly use Y
2O
2S:Eu
3+Do rouge and powder, ZnS: (Cu
2+, Al
3+) be green powder, BaMgAl
10O
17: Eu
2+Do blue powder.Yet Y
2O
2S:Eu
3+Red fluorescence powder can not well absorb in near-ultraviolet range, and its luminous efficiency is less than 1/8th of blue and green emitting phosphor, Y under this external near ultraviolet excitation
2O
2S:Eu
3+The unstable properties of red fluorescence powder, fluorescence lifetime weak point.These deficiencies of sulfide red fluorescent material become the bottleneck of white light LEDs development, silicon nitride red light emitting phosphor excellent performance, but synthetic still difficult, cost is higher.Therefore, seek a kind of low cost, high brightness, stable performance, LED red fluorescence powder that color developing is good has actual application value.
Eu
3+The tungstate red fluorescent powder that excites has many characteristics; Like its tungsten atom and four oxygen atom ligands, form tetrahedron symmetry coordinate rock steady structure, so tungstate red fluorescent powder has good chemicalstability; Sulfide or the labile deficiency of oxysulfide red fluorescence powder have been overcome; Become gradually and study also focus, rear-earth-doped in recent years tungstate red fluorescent powder has received widely and having paid close attention to, and like two times of europium ion-doped tungstate base red fluorescent powders NaLa (WO is arranged
4)
2: Eu
3+(J.Gu et al, Solid State Sciences, 2010,12,1192-1198), LiEu (WO
4)
2(J.Wang et al, Journal of Luminescence, 2006,121,57-61), KYb (WO
4)
2: Eu
3+(M.Galceran et al, Optical Materials, 2010,32,1493-1500) etc.Ji'nan University pays Qiao Ke etc. and has invented a kind of europium ion-doped ruddiness Na
5Y
1-xEu
x(WO
4)
2(MoO
4)
2Fluorescent material, its composition relative complex (one Chinese patent application number: 201110094677.2).At present less for the research report of the red fluorescence powder of rear-earth-doped basic metal four tungstate systems, its correlative study is significant.
Summary of the invention
The object of the present invention is to provide red fluorescence powder of a kind of europkium-activated four tungstate systems and preparation method thereof, the preparation of this red fluorescence powder is simple, cost is lower, luminous efficiency is high, chemicalstability is good, can effectively be excited by near-ultraviolet light or blue-light LED chip.The object of the invention is realized through following technical scheme:
A kind of is the fluorescent material of matrix with the tungstate, and said material is four wolframic acid lanthanum sodium of mixing europium, and its chemical formula is: Na
5La
1-xEu
x(WO
4)
4, wherein europium ion-doped concentration range is 0.1≤x≤1.0.
The present invention mixes the excitation spectrum of four wolframic acid lanthanum sodium of europium at 250nm-550nm, and two main absorption peaks are near 395nm and 465nm.
The mix preparation method of four wolframic acid lanthanum sodium may further comprise the steps described europium:
1. press chemical formula Na
5La
1-xEu
x(WO
4)
4Stoichiometry accurately take by weighing WO
3(99.9%), Na
2CO
3(analytical pure), Eu
2O
3(99.99%), La
2O
3(99.99%) be raw material, undertaken by following reaction formula during batching:
40WO
3+25Na
2CO
3+(5-5x)La
2O
3+5xEu
2O
3→10Na
5La
1-xEu
x(WO
4)
4+25CO
2↑
2. through high temperature solid phase synthesis, synthesize the four wolframic acid lanthanum sodium fluorescent material that obtain mixing europium.The concrete steps of high temperature solid phase synthesis are following: the reaction raw materials that will take by weighing is put into agate mortar and fully is ground to and mixes, and changes in the corundum crucible, places retort furnace to react at a certain temperature, takes out after being cooled to room temperature; The sample that takes out can obtain mixing four wolframic acid lanthanum sodium fluorescent material of europium through regrinding.
3. in the above-mentioned steps; The heating schedule of described retort furnace is that the heat-up rate with 3 ℃/min-8 ℃/min rises to 600 ℃-700 ℃; Insulation calcination 3-8 hour under this temperature stops heating after being cooled to 100 ℃ with the cooling rate of 3 ℃/min-8 ℃/min then.
4. the present invention has following characteristics:
The present invention adopts high temperature solid phase synthesis to obtain that thing phase purity is high, the four wolframic acid lanthanum sodium fluorescent material of mixing europium of better crystallinity degree, and Fig. 1 has shown its XRD figure spectrum;
The emission wavelength of fluorescent material of the present invention is in the 580nm-700nm scope, and its emission peak is in 616nm, and luminous intensity is high, and Fig. 2 has shown its emmission spectrum under the 395nm near ultraviolet excitation;
The excitation wavelength of fluorescent material of the present invention is in the 250nm-550nm scope, and two main absorption peaks can effectively be excited by near-ultraviolet light or blue-light LED chip near 395nm and 465nm;
In the fluorescent material of the present invention, the bond angle of O-W-O and Eu-O-W is bigger, at Eu
3+Between energy be difficult to take place shifts, thereby do not have the problem of concentration quenching, can realize high-concentration dopant.
The invention provides a kind of preparation method of four tungstate LED red fluorescence powders; Its technology is simple, technology maturation, production cost are lower; The very strong ruddiness of emission under the exciting of near-ultraviolet light or blue light; Having improved the colour rendering index of white light LEDs, is a kind of LED red fluorescence powder material with applications well prospect.
Description of drawings
Fig. 1 Na
5La
0.9Eu
0.1(WO
4)
4The XRD figure spectrum of fluorescent material shows that its thing phase purity is high.
Fig. 2 Na
5La
0.9Eu
0.1(WO
4)
4Fluorescent material emmission spectrum of (395nm) under near ultraviolet excitation is launched strong ruddiness.
Embodiment
Instance 1
Press chemical formula Na
5La
0.9Eu
0.1(WO
4)
4Stoichiometric, utilize the electronics Libra accurately to take by weighing WO respectively
3(99.9%), Na
2CO
3(analytical pure), Eu
2O
3(99.99%), La
2O
3(99.99%) raw material, undertaken by following reaction formula during batching:
40WO
3+25Na
2CO
3+4.5La
2O
3+0.5Eu
2O
3→10Na
5La
0.9Eu0.1(WO
4)
4+25CO
2↑
The above-mentioned raw material that takes by weighing is fully ground in agate mortar about half hour until mixing, in the corundum crucible of packing into then, and place retort furnace to heat; Utilize temperature controller that heating schedule is set; Heat-up rate with 5 ℃/min rises to 700 ℃, and insulation calcination 6 hours under this temperature is taken out sample after being cooled to room temperature with the cooling rate of 4 ℃/min then; Sample grinds to form the uniform powder of fineness once more in agate mortar, can obtain mixing four wolframic acid lanthanum sodium red fluorescence powders of europium.The XRD diffraction analysis shows that its thing phase purity is high, and fluorescence emission spectrum shows it and under near ultraviolet excitation, launches stronger ruddiness.
Instance 2
Press chemical formula Na
5La
0.8Eu
0.2(WO
4)
4Stoichiometric, utilize the electronics Libra accurately to take by weighing WO respectively
3(99.9%), Na
2CO
3(analytical pure), Eu
2O
3(99.99%), La
2O
3(99.99%) raw material adopts instance 1 similar reaction formula to carry out during batching.The above-mentioned raw material that takes by weighing is fully ground about half hour in agate mortar until mixing; Pack into then in the corundum crucible, and place retort furnace to heat, utilize temperature controller that heating schedule is set; Heat-up rate with 4 ℃/min rises to 650 ℃; Insulation calcination 7 hours under this temperature is taken out sample after being cooled to room temperature with the cooling rate of 3 ℃/min then, and sample grinds to form the uniform powder of fineness once more in agate mortar; Can obtain mixing four wolframic acid lanthanum sodium red fluorescence powders of europium, the stronger ruddiness of emission under near ultraviolet excitation.
Instance 3
Press chemical formula Na
5La
0.6Eu
0.4(WO
4)
4Stoichiometric, utilize the electronics Libra accurately to take by weighing WO respectively
3(99.9%), Na
2CO
3(analytical pure), Eu
2O
3(99.99%), La
2O
3(99.99%) raw material, distribution are similar to instance 1 and instance 2.The above-mentioned raw material that takes by weighing is handled according to instance 1 and instance 2; Heating schedule rises to 700 ℃ with the heat-up rate of 5 ℃/min; Insulation calcination 7 hours under this temperature is taken out sample after being cooled to room temperature with the cooling rate of 4 ℃/min then, and sample grinds to form the uniform powder of fineness once more in agate mortar; Can obtain mixing four wolframic acid lanthanum sodium red fluorescence powders of europium, the stronger ruddiness of emission under near ultraviolet excitation.
Instance 4
Press chemical formula Na
5La
0.4Eu
0.6(WO
4)
4Stoichiometric, utilize the electronics Libra accurately to take by weighing WO respectively
3(99.9%), Na
2CO
3(analytical pure), Eu
2O
3(99.99%), La
2O
3(99.99%) raw material adopts instance 1 similar reaction formula to carry out during batching.The raw material that takes by weighing is handled according to instance 1; Heating schedule rises to 650 ℃ with the heat-up rate of 5 ℃/min; Insulation calcination 8 hours under this temperature is taken out sample after being cooled to room temperature with the cooling rate of 3 ℃/min then, and sample grinds to form the uniform powder of fineness once more in agate mortar; Can obtain mixing four wolframic acid lanthanum sodium red fluorescence powders of europium, the stronger ruddiness of emission under near ultraviolet excitation.
Instance 5
Press chemical formula Na
5La
0.2Eu
0.8(WO
4)
4Stoichiometric, utilize the electronics Libra accurately to take by weighing WO respectively
3(99.9%), Na
2CO
3(analytical pure), Eu
2O
3(99.99%), La
2O
3(99.99%) raw material adopts instance 1 similar reaction formula to carry out during batching.The raw material that takes by weighing is handled according to instance 1; Heating schedule rises to 700 ℃ with the heat-up rate of 4 ℃/min; Insulation calcination 8 hours under this temperature is taken out sample after being cooled to room temperature with the cooling rate of 3 ℃/min then, and sample grinds to form the uniform powder of fineness once more in agate mortar; Can obtain mixing four wolframic acid lanthanum sodium red fluorescence powders of europium, the strong ruddiness of emission under near ultraviolet excitation.
Instance 6
Press chemical formula Na
5Eu (WO
4)
4Stoichiometric, utilize the electronics Libra accurately to take by weighing WO respectively
3(99.9%), Na
2CO
3(analytical pure), Eu
2O
3(99.99%) raw material adopts instance 1 similar reaction formula to carry out during batching.The raw material that takes by weighing is handled according to instance 1; Heating schedule rises to 700 ℃ with the heat-up rate of 5 ℃/min; Insulation calcination 6 hours under this temperature is taken out sample after being cooled to room temperature with the cooling rate of 4 ℃/min then, and sample grinds to form the uniform powder of fineness once more in agate mortar; Can obtain mixing four wolframic acid lanthanum sodium red fluorescence powders of europium, the strong ruddiness of emission under near ultraviolet excitation.
Instance 7
Change rare earth doped or matrix component, as mix Sm
3+Plasma can improve the luminescent properties of fluorescent material of the present invention.Based on the best Na of luminous intensity
5Eu (WO
4)
4Fluorescent material is with WO
3(99.9%), Na
2CO
3(analytical pure), Eu
2O
3(99.99%), Sm
2O
3(99.99%) is raw material,, synthesized Na according to the method for above-mentioned instance
5Eu
1-xSm
x(WO
4)
4Series phosphor powder (0.02≤x≤0.2), the fluorescence emission spectrum analysis revealed mixes Sm
3+Further strengthened the luminous intensity of fluorescent material of the present invention.
Claims (4)
1. tungstate matrix fluorescent material, said material is four wolframic acid lanthanum sodium of mixing europium, its chemical formula is Na
5La
1-xEu
x(WO
4)
4, wherein europium ion-doped concentration range is 0.1≤x≤1.0.
2. tungstate matrix fluorescent material according to claim 1 is characterized in that: change rare earth dopedly, as mix an amount of Sm
3+Ion.
3. tungstate matrix fluorescent material according to claim 1; It is characterized in that: the excitation spectrum of described fluorescent material is at 250nm～550nm; Two main absorption peaks lay respectively near 395nm and the 465nm, and its emitting fluorescence wavelength is 580nm～700nm, and peak value is near 616nm.
4. the preparation method of claim 1 or 2 or 3 described tungstate matrix fluorescent materials; Adopt high temperature solid phase synthesis; Heat-up rate with 3 ℃/min-8 ℃/min rises to 600 ℃-700 ℃, and reaction is 3-8 hour under this temperature, reduces to room temperature with the cooling rate of 3 ℃/min-8 ℃/min then.
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|---|---|---|---|
| CN201210028307.3A CN102604633B (en) | 2012-02-07 | 2012-02-07 | A kind of four tungstate red fluorescent powders and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102994083A (en) * | 2012-10-31 | 2013-03-27 | 苏州大学 | Tungstate based luminescent material as well as preparation method and application of tungstate based luminescent material |
| CN103627393A (en) * | 2013-11-19 | 2014-03-12 | 苏州大学 | Tungsten molybdate red phosphor powder and preparation method and application thereof |
| CN104818017A (en) * | 2015-03-31 | 2015-08-05 | 江苏师范大学 | Molybdate-based red fluorescent powder for white light LED and preparation method thereof |
| CN113388398A (en) * | 2021-06-11 | 2021-09-14 | 厦门理工学院 | Eu (Eu)3+Rare earth yttrium-based tungstate doped fluorescent powder and preparation method thereof |
| CN114276806A (en) * | 2022-01-28 | 2022-04-05 | 南昌工程学院 | Preparation method of fluorescent material for LED |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102994083A (en) * | 2012-10-31 | 2013-03-27 | 苏州大学 | Tungstate based luminescent material as well as preparation method and application of tungstate based luminescent material |
| CN102994083B (en) * | 2012-10-31 | 2014-05-14 | 苏州大学 | Tungstate based luminescent material as well as preparation method and application of tungstate based luminescent material |
| CN103627393A (en) * | 2013-11-19 | 2014-03-12 | 苏州大学 | Tungsten molybdate red phosphor powder and preparation method and application thereof |
| CN103627393B (en) * | 2013-11-19 | 2015-04-08 | 苏州大学 | Tungsten molybdate red phosphor powder and preparation method and application thereof |
| CN104818017A (en) * | 2015-03-31 | 2015-08-05 | 江苏师范大学 | Molybdate-based red fluorescent powder for white light LED and preparation method thereof |
| CN104818017B (en) * | 2015-03-31 | 2016-06-22 | 江苏师范大学 | Molybdate-based red fluorescent powder for white light LED and preparation method thereof |
| CN113388398A (en) * | 2021-06-11 | 2021-09-14 | 厦门理工学院 | Eu (Eu)3+Rare earth yttrium-based tungstate doped fluorescent powder and preparation method thereof |
| CN114276806A (en) * | 2022-01-28 | 2022-04-05 | 南昌工程学院 | Preparation method of fluorescent material for LED |
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|---|---|
| CN102604633B (en) | 2016-04-27 |
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