CN105199726A - NaSr2Nb5O15:xEu3<+> red phosphor powder for LED (Light Emitting Diode) and preparation method thereof - Google Patents

NaSr2Nb5O15:xEu3<+> red phosphor powder for LED (Light Emitting Diode) and preparation method thereof Download PDF

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CN105199726A
CN105199726A CN201510683750.8A CN201510683750A CN105199726A CN 105199726 A CN105199726 A CN 105199726A CN 201510683750 A CN201510683750 A CN 201510683750A CN 105199726 A CN105199726 A CN 105199726A
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powder
led
red fluorescence
nasr
xeu
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宁青菊
曹舒尧
姜佳敏
史永胜
于成龙
刘波
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a preparation method of NaSr2Nb5O15:xEu3<+> red phosphor powder for an LED (Light Emitting Diode), and belongs to the technical field of preparation of luminescent materials. The method comprises the following steps: uniformly grinding and mixing Sr(NO3)2, Nb2O5 and Eu2O3, serving as raw materials, by using fused salt NaCl, Na2CO3 and KNO3 as reaction media, and then preparing a NaSr2Nb5O15:xEu3<+> phosphor powder body at a lower temperature by using a salt fusion method (compared with a solid phase method), where x is equal to 0.005 to 0.05. The NaSr2Nb5O15:xEu3<+> red phosphor powder prepared by using the preparation method can achieve the generation of red light which is stable and efficient under ultraviolet-near ultraviolet excitation.

Description

A kind of LED NaSr 2nb 5o 15: xEu 3+red fluorescence powder and preparation method thereof
Technical field
The invention belongs to luminescent material preparing technical field, relate to a kind of preparation method of red fluorescence powder, be specifically related to a kind of LED NaSr 2nb 5o 15: xEu 3+red fluorescence powder and preparation method thereof.
Background technology
White light LEDs has the features such as energy-saving and environmental protection, efficient, easy care, life-span be long because of it, has been widely used in display and lighting field.At present, high-quality white light LEDs realizes white light emission two kinds of major ways: one, is utilize blue chip to excite yellow fluorescent powder, realizes white light emission by remaining blue light and gold-tinted compound; Its two, be utilize ultraviolet-near ultraviolet chip to excite red-green-blue fluorescent material, realize white light emission by three primary colours photorecombination.But the former is owing to lacking red color light component, make colour rendering index low, color reducibility is poor, and the latter is limited to and lacks at present and can be produced the fluorescent material of efficient red emission under ultraviolet-near ultraviolet excitation.Therefore, develop ultraviolet-near ultraviolet excitated lower fluorescent material tool that can produce efficient stable red emission to be of great significance.
Fluorescent material matrix compounds scope is very wide, comprises silicate, phosphoric acid salt, borate, vanadate, aluminate, niobate etc.Wherein, niobate has that receptivity is strong, efficiency of conversion is high, have the advantages such as good fluorescent emission efficiency in visible region.Therefore, niobate is a kind of substrate material of luminescent properties excellence.
The common synthesis technique of niobate has solid reaction process, chemical precipitation method, hydrothermal synthesis method etc.Adopt fluorescent material prepared by solid phase method, sintering temperature is higher, and granularity is comparatively large, and size distribution is uneven, is difficult to obtain spheroidal particle, is not easy to coating; The purity requirement of chemical precipitation method to raw material is higher, and in preparation process, chemical reaction is complicated, easily introduces impurity, thus affects the luminescent properties of fluorescent material; Hydrothermal method, owing to being only applicable to the preparation of oxide compound or the water insensitive sulfide of minority, has significant limitation.The luminescent properties of fluorescent material, mostly by the impact of fluorescent material purity, granularity and particle size uniformity, so the fluorescent material matrix of high purity, uniform crystalline phase is more conducive to the luminescent properties improving fluorescent material.
Summary of the invention
In order to overcome the defect that above-mentioned prior art exists, the object of the present invention is to provide a kind of LED NaSr 2nb 5o 15: xEu 3+red fluorescence powder and preparation method thereof, the method is simple to operate, environmental protection; Obtained NaSr 2nb 5o 15: xEu 3+red fluorescence powder purity is high, epigranular, crystal property are good.
The present invention is achieved through the following technical solutions:
The invention discloses a kind of LED NaSr 2nb 5o 15: xEu 3+the preparation method of red fluorescence powder, comprises the following steps:
1) by 2:(2.75 ~ 3.25): the mol ratio of (0.0025 ~ 0.025), get Sr (NO respectively 3) 2, Nb 2o 5and Eu 2o 3, after mixing, grinding evenly, obtains material powder;
2) by (0.5 ~ 1.5): (0.25 ~ 0.75): the mol ratio of 1, takes NaCl, Na respectively 2cO 3and KNO 3, after mixing, grinding evenly, obtains fused salt powder;
3), by (0.5 ~ 4): the mass ratio of 1, after being mixed with fused salt powder by material powder, grinding evenly, obtains mixed powder;
4) mixed powder is placed in crucible, from room temperature, with 2 DEG C/min ramp to 150 ~ 200 DEG C, again with 3 DEG C/min ramp to 200 ~ 600 DEG C, then with 5 DEG C/min ramp to 900 ~ 1300 DEG C, after insulation 2 ~ 24h, be cooled to 500 DEG C with 5 DEG C/min speed, finally cool to room temperature with the furnace;
5) by step 4) process after product cleaning until removing fused salt, by product dry, grinding, obtained LED NaSr 2nb 5o 15: xEu 3+red fluorescence powder, wherein, x=0.005 ~ 0.05.
Step 1), 2), 3) all adopt agate mortar raw material is ground, milling time is 20 ~ 40min.
Step 5) be adopt deionized water to step 4) process after product repeatedly soak, carrying out washing treatment.
Step 5) adopt Silver Nitrate inspection washing clear liquid, until without precipitation in washing clear liquid.
The invention also discloses the LED red fluorescence powder adopting aforesaid method obtained, the chemical constitution of this red fluorescence powder is: NaSr 2nb 5o 15: xEu 3+, wherein, x=0.005 ~ 0.05.
The powder purity of described red fluorescence powder reaches 100%, and median size is 10 ~ 16 μm, and red light color purity reaches more than 90%.
Compared with prior art, the present invention has following useful technique effect:
LED NaSr disclosed by the invention 2nb 5o 15: xEu 3+the preparation method of red fluorescence powder, with Sr (NO 3) 2, Nb 2o 5, Eu 2o 3for raw material, adopt fused salt NaCl, Na 2cO 3, KNO 3as reaction medium, after being ground, (compared with solid phase method) realizes fluorescent material NaSr at a lower temperature 2nb 5o 15: xEu 3+the molten-salt growth method preparation of (wherein x=0.005 ~ 0.05) powder.Through the NaSr that the present invention obtains 2nb 5o 15: xEu 3+red fluorescence powder can realize the ruddiness at ultraviolet-near ultraviolet excitated lower generation stability and high efficiency.
Through XRD, SEM and spectrophotofluorometer testing and analyzing, the NaSr that the present invention obtains 2nb 5o 15: xEu 3+red fluorescence powder powder purity up to 100%, good, the uniform particle sizes of crystal property and favorable dispersity, median size is 10 ~ 16 μm, red light color high purity more than 90%, and optimum CIE chromaticity coordinates is positioned at (0.628,0.371) place, close with standard red spot.
Accompanying drawing explanation
Fig. 1 is the NaSr that the embodiment of the present invention 1 obtains 2nb 5o 15: xEu 3+the XRD figure of fluorescent material;
Fig. 2 is the NaSr that the embodiment of the present invention 2 obtains 2nb 5o 15: xEu 3+the utilizing emitted light spectrogram of fluorescent material;
Fig. 3 is the NaSr that the embodiment of the present invention 4 obtains 2nb 5o 15: xEu 3+the CIE figure of fluorescent material.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail:
Embodiment 1
1) according to the mol ratio of 2:2.875:0.0025, Sr (NO is taken respectively 3) 2, Nb 2o 5, Eu 2o 3raw material is placed in agate mortar 1, and raw material is at room temperature ground 30min, and raw material is mixed;
2) according to the mol ratio of 1.5:0.75:1, NaCl, Na is taken respectively 2cO 3, KNO 3be placed in agate mortar 2 as fused salt, fused salt is at room temperature ground 30min, make two kinds of salt material Homogeneous phase mixing;
3) according to the mass ratio of 2.5:1, take step one gained material powder respectively and step 2 gained fused salt is placed in agate mortar 3, mixture is at room temperature ground in 30min, makes raw material and fused salt Homogeneous phase mixing;
4) step 3 mixture is placed in crucible, from room temperature, with 2 DEG C/min ramp to 180 DEG C, again with 3 DEG C/min ramp to 400 DEG C, then with 5 DEG C/min ramp to 1000 DEG C, at 1000 DEG C, be incubated 12h, be cooled to 500 DEG C with 3 DEG C/min speed, after cool to room temperature with the furnace;
5) step 4 products therefrom deionized water is repeatedly soaked, washs, with Silver Nitrate inspection washing clear liquid, until after removing fused salt completely, product dried, grind, namely obtain NaSr 2nb 5o 15: xEu 3+fluorescent material, wherein x=0.005.
See Fig. 1, be the NaSr that the present embodiment is obtained 2nb 5o 15: xEu 3+the XRD figure of fluorescent material, as can be seen from the figure, the XRD diffraction peak of prepared sample and standard card (No.34-0429) substantially identical, Eu 3+doping do not introduce dephasign, show that obtained sample is highly purified single-phase, and Eu 3+successfully be mixed with in parent lattice.
Embodiment 2
1) according to the mol ratio of 2:2.75:0.0075, Sr (NO is taken respectively 3) 2, Nb 2o 5, Eu 2o 3raw material is placed in agate mortar 1, and raw material is at room temperature ground 30min, and raw material is mixed;
2) according to the mol ratio of 1:0.5:1, NaCl, Na is taken respectively 2cO 3, KNO 3be placed in agate mortar 2 as fused salt, fused salt is at room temperature ground 30min, make two kinds of salt material Homogeneous phase mixing;
3) according to the mass ratio of 3.5:1, take step one gained material powder respectively and step 2 gained fused salt is placed in agate mortar 3, mixture is at room temperature ground in 30min, makes raw material and fused salt Homogeneous phase mixing;
4) step 3 mixture is placed in crucible, from room temperature, with 2 DEG C/min ramp to 150 DEG C, again with 3 DEG C/min ramp to 200 DEG C, then with 5 DEG C/min ramp to 1300 DEG C, at 1300 DEG C, be incubated 18h, be cooled to 500 DEG C with 2 DEG C/min speed, after cool to room temperature with the furnace;
5) step 4 products therefrom deionized water is repeatedly soaked, washs, with Silver Nitrate inspection washing clear liquid, until after removing fused salt completely, product dried, grind, namely obtain NaSr 2nb 5o 15: xEu 3+red fluorescence powder, wherein x=0.015.
See Fig. 2, be the NaSr that the present embodiment is obtained 2nb 5o 15: xEu 3+the utilizing emitted light spectrogram of fluorescent material, as can be seen from the figure, the NaSr prepared by embodiment 2 2nb 5o 15: xEu 3+fluorescent material is under wavelength is the near ultraviolet excitation of 399nm, and its two main emission peaks lay respectively at 616nm place and 595nm place, correspond respectively to Eu 3+'s 5d 0→ 7f 2and 5d 0→ 7f 1characteristic transition, other position emission peak is less and peak intensity is more weak, shows that the fluorescent material prepared by embodiment 2 is under the near ultraviolet excitation of 399nm at wavelength, can launch strong ruddiness, and without the light emission of other color.
Embodiment 3
1) according to the mol ratio of 2:3:0.025, Sr (NO is taken respectively 3) 2, Nb 2o 5, Eu 2o 3raw material is placed in agate mortar 1, and raw material is at room temperature ground 30min, and raw material is mixed;
2) according to the mol ratio of 1.5:0.5:1, NaCl, Na is taken respectively 2cO 3, KNO 3be placed in agate mortar 2 as fused salt, fused salt is at room temperature ground 30min, make two kinds of salt material Homogeneous phase mixing;
3) according to the mass ratio of 0.5:1, take step one gained material powder respectively and step 2 gained fused salt is placed in agate mortar 3, mixture is at room temperature ground in 30min, makes raw material and fused salt Homogeneous phase mixing;
4) step 3 mixture is placed in crucible, from room temperature, with 2 DEG C/min ramp to 150 DEG C, again with 3 DEG C/min ramp to 200 DEG C, then with 5 DEG C/min ramp to 1100 DEG C, at 1100 DEG C, be incubated 2h, be cooled to 500 DEG C with 3 DEG C/min speed, after cool to room temperature with the furnace;
5) step 4 products therefrom deionized water is repeatedly soaked, washs, with Silver Nitrate inspection washing clear liquid, until after removing fused salt completely, product dried, grind, namely obtain NaSr 2nb 5o 15: xEu 3+red fluorescence powder, wherein x=0.05.
Embodiment 4
1) according to the mol ratio of 2:3.25:0.0125, Sr (NO is taken respectively 3) 2, Nb 2o 5, Eu 2o 3raw material is placed in agate mortar 1, and raw material is at room temperature ground 30min, and raw material is mixed;
2) according to the mol ratio of 0.5:0.25:1, NaCl, Na is taken respectively 2cO 3, KNO 3be placed in agate mortar 2 as fused salt, fused salt is at room temperature ground 30min, make two kinds of salt material Homogeneous phase mixing;
3) according to the mass ratio of 1.5:1, take step one gained material powder respectively and step 2 gained fused salt is placed in agate mortar 3, mixture is at room temperature ground in 30min, makes raw material and fused salt Homogeneous phase mixing;
4) step 3 mixture is placed in crucible, from room temperature, with 2 DEG C/min ramp to 200 DEG C, again with 3 DEG C/min ramp to 600 DEG C, then with 5 DEG C/min ramp to 1200 DEG C, at 1200 DEG C, be incubated 6h, be cooled to 500 DEG C with 5 DEG C/min speed, after cool to room temperature with the furnace;
5) step 4 products therefrom deionized water is repeatedly soaked, washs, with Silver Nitrate inspection washing clear liquid, until after removing fused salt completely, product dried, grind, namely obtain NaSr 2nb 5o 15: xEu 3+red fluorescence powder, wherein x=0.025.
See Fig. 3, be the NaSr that the present embodiment is obtained 2nb 5o 15: xEu 3+the CIE figure of fluorescent material, as can be seen from the figure, the chromaticity coordinates of the ruddiness that the sample prepared by embodiment 4 is launched under the near ultraviolet excitation of wavelength for 399nm is positioned at (0.6149,0.3462), be near the mark red spot, and colour temperature reaches 1150k, shows that the sample prepared by embodiment 4 is can send the higher warm ruddiness of purity under the near ultraviolet excitation of 399nm at wavelength, may be used for white light LEDs, to improve colour temperature.
Embodiment 5
1) according to the mol ratio of 2:3.125:0.02, Sr (NO is taken respectively 3) 2, Nb 2o 5, Eu 2o 3raw material is placed in agate mortar 1, and raw material is at room temperature ground 30min, and raw material is mixed;
2) according to the mol ratio of 1:0.25:1, NaCl, Na is taken respectively 2cO 3, KNO 3be placed in agate mortar 2 as fused salt, fused salt is at room temperature ground 30min, make two kinds of salt material Homogeneous phase mixing;
3) according to the mass ratio of 4:1, take step one gained material powder respectively and step 2 gained fused salt is placed in agate mortar 3, mixture is at room temperature ground in 30min, makes raw material and fused salt Homogeneous phase mixing;
4) step 3 mixture is placed in crucible, from room temperature, with 2 DEG C/min ramp to 160 DEG C, again with 3 DEG C/min ramp to 500 DEG C, then with 5 DEG C/min ramp to 900 DEG C, at 900 DEG C, be incubated 24h, be cooled to 500 DEG C with 4 DEG C/min speed, after cool to room temperature with the furnace;
5) step 4 products therefrom deionized water is repeatedly soaked, washs, with Silver Nitrate inspection washing clear liquid, until after removing fused salt completely, product dried, grind, namely obtain NaSr 2nb 5o 15: xEu 3+red fluorescence powder, wherein x=0.025.

Claims (6)

1. a LED NaSr 2nb 5o 15: xEu 3+the preparation method of red fluorescence powder, is characterized in that, comprises the following steps:
1) by 2:(2.75 ~ 3.25): the mol ratio of (0.0025 ~ 0.025), get Sr (NO respectively 3) 2, Nb 2o 5and Eu 2o 3, after mixing, grinding evenly, obtains material powder;
2) by (0.5 ~ 1.5): (0.25 ~ 0.75): the mol ratio of 1, takes NaCl, Na respectively 2cO 3and KNO 3, after mixing, grinding evenly, obtains fused salt powder;
3), by (0.5 ~ 4): the mass ratio of 1, after being mixed with fused salt powder by material powder, grinding evenly, obtains mixed powder;
4) mixed powder is placed in crucible, from room temperature, with 2 DEG C/min ramp to 150 ~ 200 DEG C, again with 3 DEG C/min ramp to 200 ~ 600 DEG C, then with 5 DEG C/min ramp to 900 ~ 1300 DEG C, after insulation 2 ~ 24h, be cooled to 500 DEG C with 5 DEG C/min speed, finally cool to room temperature with the furnace;
5) by step 4) process after product cleaning until removing fused salt, by product dry, grinding, obtained LED NaSr 2nb 5o 15: xEu 3+red fluorescence powder, wherein, x=0.005 ~ 0.05.
2. LED NaSr according to claim 1 2nb 5o 15: xEu 3+the preparation method of red fluorescence powder, is characterized in that, step 1), 2), 3) all adopt agate mortar raw material is ground, milling time is 20 ~ 40min.
3. LED NaSr according to claim 1 2nb 5o 15: xEu 3+the preparation method of red fluorescence powder, is characterized in that, step 5) be adopt deionized water to step 4) process after product repeatedly soak, carrying out washing treatment.
4. LED NaSr according to claim 1 2nb 5o 15: xEu 3+the preparation method of red fluorescence powder, is characterized in that, step 5) adopt Silver Nitrate inspection washing clear liquid, until without precipitation in washing clear liquid.
5. adopt the LED red fluorescence powder that the method in Claims 1 to 4 described in any one is obtained, it is characterized in that, the chemical constitution of this red fluorescence powder is: NaSr 2nb 5o 15: xEu 3+, wherein, x=0.005 ~ 0.05.
6. LED red fluorescence powder according to claim 5, is characterized in that, the powder purity of described red fluorescence powder reaches 100%, and median size is 10 ~ 16 μm, and red light color purity reaches more than 90%.
CN201510683750.8A 2015-10-20 2015-10-20 NaSr2Nb5O15:xEu3<+> red phosphor powder for LED (Light Emitting Diode) and preparation method thereof Pending CN105199726A (en)

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Publication number Priority date Publication date Assignee Title
CN106566544A (en) * 2016-11-09 2017-04-19 广东省稀有金属研究所 Nitric oxide red fluorescence material

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106566544A (en) * 2016-11-09 2017-04-19 广东省稀有金属研究所 Nitric oxide red fluorescence material
CN106566544B (en) * 2016-11-09 2019-04-19 广东省稀有金属研究所 A kind of nitrogen oxides red fluorescence material

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