CN103992795B - A kind of LED red fluorescence powder and preparation method thereof - Google Patents

A kind of LED red fluorescence powder and preparation method thereof Download PDF

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CN103992795B
CN103992795B CN201410183921.6A CN201410183921A CN103992795B CN 103992795 B CN103992795 B CN 103992795B CN 201410183921 A CN201410183921 A CN 201410183921A CN 103992795 B CN103992795 B CN 103992795B
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red fluorescence
fluorescence powder
led red
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led
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CN103992795A (en
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张君诚
韩文鹏
龙云泽
孟超
张国首
刘凯月
刘艳杰
辛星
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Qingdao University
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Abstract

LED red fluorescence powder disclosed by the invention is the alkaline earth metal niobate fluorescent material that praseodymium activates, and its chemical expression is (Ca 1-x-y-2zsr xba ya zpr z) 2nb 2o7, wherein A represents monovalent base metallic element, is selected from least one in Li, Na, K and Rb; 0≤x≤0.2; 0≤y≤0.1; 0 < z≤0.05.This fluorescent material is prepared: according to chemical expression metering than the compound taken containing respective element by high temperature solid-state method, mixed grinding evenly and dry, after pre-burning under air or oxygen environment, high-temperature calcination, then through pulverizing, grinding, clean removal of impurities, drying and processing.Not only preparation method is simple, pollution-free for this fluorescent material, cost is low, and there is the advantages such as excitation wavelength range is wide, good luminescence property, colour rendering index are high, temperature stability good, moistureproof, UV-light or blue-light LED chip manufacture white light LEDs can be widely used in.

Description

A kind of LED red fluorescence powder and preparation method thereof
Technical field
The present invention relates to alkaline earth metal niobate red fluorescence powder of a kind of praseodymium activation and preparation method thereof, red fluorescence powder being particularly useful for LED and preparation method thereof, belongs to rare earth luminescent material technical field.
Background technology
The nineties in 20th century, along with the appearance of GaN, InGaN base blueness (450 ~ 470nm) and near ultraviolet (380 ~ 410nm) photodiode (LED), there is the white light LEDs being combined by blue or near ultraviolet LED chip and light conversion phosphor and made.This novel solid light source is compared to traditional incandescent light, luminescent lamp and high voltage mercury lamp, there is the plurality of advantages such as efficient energy-saving, environmental protection, life-span long (more than 10000 hours), volume are little, huge application prospect is had in illumination and display field, be expected to realize industrialization, substitute existing lighting fixtures, become forth generation lighting source.
Adopt LED chip and phosphor combination to produce white light and have three kinds of modes: blue LED die and yellow fluorescent powder combine; Blue LED die combines with red, green emitting phosphor; Near ultraviolet or purple LED chip and red, green, blue three primary colors fluorescent powder combine.Current employing blue light GaN or InGaN base LED chip coating yellow fluorescent powder Y 3al 5o 12: Ce 3+(YAG:Ce) high-brightness white-light LED made realizes commercialization, and enters special lighting field.But there is the lower inherent defect of colour rendering index because lacking red spectral band transmitting in this product, need add red fluorescence powder to obtain high colour rendering index, can be applied to general illumination occasion.In addition, other two kinds of combinations also need the cooperation of the high quality red fluorescent powder that can be excited by blueness, purple or near ultraviolet LED, could realize the better color developing of white light LEDs and any coupling of colour temperature within the scope of 2500 ~ 10000K thereof.In prior art, commercial red fluorescence powder mainly contains (Ca, Sr) S:Eu 2+, Y 2o 3: Eu 2+, (Y, Gd) BO 3: Eu 3+deng, but these fluorescent material or poor stability, easily deliquescence, need carry out coated process during use, also or luminous efficiency not high, cause that the white light LEDs colour rendering index that encapsulates out is not high or efficiency is not high.
Therefore, in order to obtain the white light LEDs of high-level efficiency, high color rendering index (CRI), high stability, this will ask for help develop the red fluorescent powder for white radiation LED with more premium properties.The calcium niobate of non-doped with rare-earth elements itself is a kind of piezoelectricity, photoelectricity, ferroelectric material of high-quality, has good moistureproofness, thermostability and chemical stability.The present invention is the requirement adapting to White light LED technology development, develops alkaline earth metal niobate red fluorescence powder that a kind of praseodymium for white light LEDs activates and preparation method thereof.
Summary of the invention
The object of the present invention is to provide one can be excited by UV-light or blue-ray LED, there is good luminous characteristic and physicochemical characteristic, and LED red fluorescence powder that preparation method is simple, pollution-free, cost is low and preparation method thereof, to overcome problems of the prior art.
To achieve these goals, the present invention realizes by the following technical solutions:
LED red fluorescence powder of the present invention is the alkaline earth metal niobate fluorescent material that praseodymium activates, and its chemical expression is (Ca 1-x-y-2zsr xba ya zpr z) 2nb 2o 7, wherein A represents monovalent base metallic element, is selected from least one in Li, Na, K and Rb; 0≤x≤0.2; 0≤y≤0.1; 0 < z≤0.1.
Preferably, the span of described x is 0≤x≤0.1.
Preferably, the span of described y is 0≤y≤0.05.
Preferably, the span of described z is 0.01≤z≤0.05.
Wherein, A as valence state compensating elements, for compensate trivalent rare earth praseodymium ion substitute divalent alkaline-earth metal ion after electric charge do not mate, thus reach minimizing fault in material, improve the object of luminous intensity.
The preparation method of LED red fluorescence powder of the present invention, comprises following processing step:
(1) measure than the raw materials of compound taken containing Elements C a, Sr, Ba, Pr, Nb and A by element chemistry, add deionized water or dehydrated alcohol grinding, mix, dry in 50 ~ 100 DEG C of baking ovens and obtain mixed powder;
(2) by the pre-burning at 800 ~ 1000 DEG C in air or oxygen of the mixed powder of step (1) gained, pre-burning soaking time is 1 ~ 5 hour;
(3), after being ground by cooled pre-burning product, calcine at 1200 ~ 1450 DEG C in air or oxygen, the sintering soak time is 2 ~ 10 hours;
(4) carry out pulverizing after calcinate cooling step (3) obtained, grind, clean removal of impurities, oven dry, namely obtain LED red fluorescence powder.
The raw materials of compound containing Elements C a, Sr, Ba, Pr, Nb and A described in the present invention is selected from the oxide compound of Ca, Sr, Ba, Pr, Nb and A, oxyhydroxide, carbonate, nitrate, oxalate, acetate.
In above-mentioned steps (1), during grinding, the mass ratio of deionized water or dehydrated alcohol and raw mixture is 1: 1 ~ 3: 1, and milling time is 1 ~ 10 hour.
In above-mentioned steps (4), pulverizing can adopt the broken or comminution by gas stream of physics, cleaning comprise in washing, pickling or alkali cleaning one or more.
In above-mentioned steps (4), the mean particle size of obtained LED red fluorescence powder is 0.1 ~ 30 μm.
Feature of the present invention is:
(1) the LED red fluorescence powder, preparation method thereof that the present invention relates to is simple, pollution-free, cost is low.
(2) the LED red light emitting phosphor excellent property that obtains of the present invention, has higher colour rendering index, good to the temperature stability under 300 DEG C of conditions in room temperature, and physicochemical property are stablized, water-fast protection against the tide.
(3) the LED red fluorescence powder excitation wavelength range that obtains of the present invention is wide, comprise the UV-light wave band of 200 ~ 400nm and the blue wave band of 430 ~ 510nm, wherein, the excitation peak of UV-light wave band is positioned at 311nm, and the excitation peak of blue wave band is positioned at 457nm, 476nm and 493nm.Current mature InGaN blue LED die emmission spectrum scope is at 430 ~ 500nm, and emission peak is positioned at 460 ± 10nm, fully mates with the excitation peak of LED red fluorescence powder blue wave band of the present invention.The emission peak wavelength of LED red fluorescence powder of the present invention, at 590 ~ 650nm, is launched main peak and is positioned at 614nm, can make up well in current white light LEDs to lack red spectral band or red spectral band and launch more weak deficiency.
(4) the LED red fluorescence powder that obtains of the present invention, can combine with green emitting phosphor, be coated on blue LED die, prepare white light LEDs; Or coordinate with ultraviolet leds, the preparation of white light LEDs is used for as red fluorescence part; Also or with UV-light, blue-ray LED coordinate, combine with other color fluorescence powder, prepare the color LED that color is different.
Accompanying drawing explanation
Fig. 1 is Ca 2nb 2o 7powdery diffractometry standard card (18-0301) and embodiment 1 sample (Ca 0.98k 0.01pr 0.01) 2nb 2o 7x-ray powder diffraction figure.
Fig. 2 is monitoring embodiment 1 sample (Ca 0.98k 0.01pr 0.01) 2nb 2o 7the exciting light spectrogram of 614nm red emission.
Fig. 3 is 311nm ultraviolet excitation embodiment 1 sample (Ca 0.98k 0.01pr 0.01) 2nb 2o 7the utilizing emitted light spectrogram obtained.
Fig. 4 is 457nm blue-light excited embodiment 1 sample (Ca 0.98k 0.01pr 0.01) 2nb 2o 7the utilizing emitted light spectrogram obtained.
Fig. 5 is 476nm blue-light excited embodiment 1 sample (Ca 0.98k 0.01pr 0.01) 2nb 2o 7the utilizing emitted light spectrogram obtained.
Fig. 6 is 493nm blue-light excited embodiment 1 sample (Ca 0.98k 0.01pr 0.01) 2nb 2o 7the utilizing emitted light spectrogram obtained.
Fig. 7 is the comparison diagram of the relative luminous intensity (excitation wavelength is 457nm) of embodiment 1-8 sample.
Specific embodiments
Below by way of particular specific embodiment, also the present invention will be described in more detail by reference to the accompanying drawings.Should be understood that one or more method stepss that the present invention mentions do not repel also there is other method steps before and after described combination step, or other method steps can also be inserted before these steps clearly mentioned; Should also be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.And, except as otherwise noted, the numbering of various method steps is only the convenient tool differentiating various method steps, but not be ordering or the enforceable scope of restriction the present invention of restriction various method steps, the change of its relativeness or adjustment, when changing technology contents without essence, when being also considered as the enforceable category of the present invention.
Embodiment 1
(Ca 0.98k 0.01pr 0.01) 2nb 2o 7the preparation of sample:
(1) raw materials of Ca CO is taken 37.8392g, K 2cO 30.055g, Pr 6o 110.1361g, Nb 2o 510.6277g, above raw material is analytical pure, puts into agate mortar and adds after 30g dehydrated alcohol grinds 2 hours, dry in 60 DEG C of baking ovens;
(2) mixed powder after drying to be placed in alumina crucible in air atmosphere at 900 DEG C pre-burning 4 hours;
(3) preburning powdered material after grinding is calcined 4 hours in air atmosphere at 1400 DEG C;
(4) by cooled product physical fragmentation, grinding, ion, oven dry, chemical constitution is namely obtained for (Ca 0.98k 0.01pr 0.01) 2nb 2o 7lED red fluorescence powder.
The LED red fluorescence powder outward appearance that this embodiment is prepared is in white, and X-ray powder diffraction (XRD) test shows, as shown in Figure 1, and the diffraction peak data of gained sample and Ca 2nb 2o 7the diffraction data of powdery diffractometry standard card (18-0301) is consistent, and without dephasign, illustrates that gained sample is pure phase Ca 2nb 2o 7structure.As shown in Figure 2, its excitation wavelength range is wide for the excitation spectrum of monitoring 614nm red emission, comprises excitation peak and is positioned at 430 ~ 510nm blue wave band that 200 ~ 400nm UV-light wave band of 311nm and excitation peak are positioned at 457nm, 476nm and 493nm.Current mature InGaN blue LED die emmission spectrum scope is at 430 ~ 500nm, and emission peak is positioned at 460 ± 10nm, fully mates with the excitation peak of fluorescent material blue wave band of the present invention.Fig. 3 ~ Fig. 6 sets forth the emmission spectrum of LED red fluorescence powder under 311nm UV-light, 457nm blue light, 476nm blue light and 493nm are blue-light excited that this embodiment is prepared.As seen from the figure, the emission wavelength ranges of this fluorescent material, at 590 ~ 650nm, launches main peak at 614nm, can make up well in current white light LEDs to lack red spectral band or red spectral band and launch more weak deficiency.The exciting peak position, launch peak position of the LED red fluorescence powder that this embodiment obtains, calcination atmosphere, calcining temperature, granularity data are as shown in table 1.
Embodiment 2
(Ca 0.97na 0.015pr 0.015) 2nb 2o 7the preparation of sample:
(1) raw materials of Ca CO is taken 37.7592g, Na 2cO 30.0633g, Pr 6o 110.2041g, Nb 2o 510.6277g, above raw material is analytical pure, puts into agate mortar and adds after 25g dehydrated alcohol grinds 1.5 hours, dry in 70 DEG C of baking ovens;
(2) mixed powder after drying to be placed in alumina crucible in air atmosphere at 850 DEG C pre-burning 4 hours;
(3) preburning powdered material after grinding is calcined 6 hours in air atmosphere at 1350 DEG C;
(4) by cooled product physical fragmentation, grinding, ion, oven dry, chemical constitution is namely obtained for (Ca 0.97na 0.015pr 0.015) 2nb 2o 7lED red fluorescence powder.
The obtained LED of this embodiment is by red fluorescence powder outward appearance in white, and XRD spectra result is basically identical with embodiment 1, and it excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1.
Embodiment 3
(Ca 0.93sr 0.05k 0.01pr 0.01) 2nb 2o 7the preparation of sample:
(1) raw materials of Ca CO is taken 37.4392g, SrCO 30.5899g, K 2cO 30.055g, Pr 6o 110.1361g, Nb 2o 510.6277g, above raw material is analytical pure, puts into agate mortar and adds after 35g deionized water grinds 2.5 hours, dry in 80 DEG C of baking ovens;
(2) mixed powder after drying to be placed in alumina crucible in air atmosphere at 850 DEG C pre-burning 5 hours;
(3) preburning powdered material after grinding is calcined 8 hours in oxygen atmosphere at 1350 DEG C;
(4) by cooled product physical fragmentation, grinding, ion, oven dry, chemical constitution is namely obtained for (Ca 0.93sr 0.05k 0.01pr 0.01) 2nb 2o 7lED red fluorescence powder.
The obtained LED of this embodiment is by red fluorescence powder outward appearance in white, and XRD spectra result is basically identical with embodiment 1, and it excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1.
Embodiment 4
(Ca 0.93ba 0.05li 0.01pr 0.01) 2nb 2o 7the preparation of sample:
(1) raw materials of Ca CO is taken 37.4392g, BaCO 30.7886g, Li 2cO 30.0294g, Pr 6o 110.1361g, Nb 2o 510.6277g, above raw material is analytical pure, puts into agate mortar and adds after 20g dehydrated alcohol grinds 2 hours, dry in 50 DEG C of baking ovens;
(2) mixed powder after drying to be placed in alumina crucible in air atmosphere at 900 DEG C pre-burning 4 hours;
(3) preburning powdered material after grinding is calcined 5 hours in oxygen atmosphere at 1380 DEG C;
(4) by cooled product physical fragmentation, grinding, ion, oven dry, chemical constitution is namely obtained for (Ca 0.93ba 0.05li 0.01pr 0.01) 2nb 2o 7lED red fluorescence powder.
The obtained LED of this embodiment is by red fluorescence powder outward appearance in white, and XRD spectra result is basically identical with embodiment 1, and it excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1.
Embodiment 5
(Ca 0.86sr 0.1na 0.01k 0.01pr 0.02) 2nb 2o 7the preparation of sample:
(1) raw materials of Ca CO is taken 36.8793g, SrCO 31.1799g, Na 2cO 30.0422g, K 2cO 30.055g, Pr 6o 110.2721g, Nb 2o 510.6277g, above raw material is analytical pure, puts into agate mortar and adds after 20g deionized water grinds 1.5 hours, dry in 80 DEG C of baking ovens;
(2) mixed powder after drying to be placed in alumina crucible in air atmosphere at 850 DEG C pre-burning 5 hours;
(3) preburning powdered material after grinding is calcined 8 hours in oxygen atmosphere at 1300 DEG C;
(4) by cooled product physical fragmentation, grinding, ion, oven dry, chemical constitution is namely obtained for (Ca 0.86sr 0.1na 0.01k 0.01pr 0.02) 2nb 2o 7lED red fluorescence powder.
The obtained LED of this embodiment is by red fluorescence powder outward appearance in white, and XRD spectra result is basically identical with embodiment 1, and it excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1.
Embodiment 6
(Ca 0.9sr 0.04ba 0.02na 0.02pr 0.02) 2nb 2o 7the preparation of sample:
(1) raw materials of Ca CO is taken 37.1993g, SrCO 30.4719g, BaCO 30.3154g, Na 2cO 30.0844g, Pr 6o 110.2721g, Nb 2o 510.6277g, above raw material is analytical pure, puts into agate mortar and adds after 40g deionized water grinds 3 hours, dry in 80 DEG C of baking ovens;
(2) mixed powder after drying to be placed in alumina crucible in oxygen atmosphere at 900 DEG C pre-burning 6 hours;
(3) preburning powdered material after grinding is calcined 8 hours in oxygen atmosphere at 1350 DEG C;
(4) by cooled product physical fragmentation, grinding, ion, oven dry, chemical constitution is namely obtained for (Ca 0.9sr 0.04ba 0.02na 0.02pr 0.02) 2nb 2o 7lED red fluorescence powder.
The obtained LED of this embodiment is by red fluorescence powder outward appearance in white, and XRD spectra result is basically identical with embodiment 1, and it excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1.
Embodiment 7
(Ca 0.86sr 0.05ba 0.05na 0.01k 0.01pr 0.02) 2nb 2o 7the preparation of sample:
(1) raw materials of Ca CO is taken 36.8793g, SrCO 30.5899g, BaCO 30.7886g, Na 2cO 30.0422g, K 2cO 30.055g, Pr 6o 110.2721g, Nb 2o 510.6277g, above raw material is analytical pure, puts into agate mortar and adds after 40g dehydrated alcohol grinds 3 hours, dry in 50 DEG C of baking ovens;
(2) mixed powder after drying to be placed in alumina crucible in oxygen atmosphere at 850 DEG C pre-burning 5 hours;
(3) preburning powdered material after grinding is calcined 5 hours in oxygen atmosphere at 1390 DEG C;
(4) by cooled product physical fragmentation, grinding, ion, oven dry, chemical constitution is namely obtained for (Ca 0.86sr 0.05ba 0.05na 0.01k 0.01pr 0.02) 2nb 2o 7lED red fluorescence powder.
The obtained LED of this embodiment is by red fluorescence powder outward appearance in white, and XRD spectra result is basically identical with embodiment 1, and it excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1.
Embodiment 8
(Ca 0.84sr 0.06ba 0.04li 0.01na 0.01k 0.01pr 0.03) 2nb 2o 7the preparation of sample:
(1) raw materials of Ca CO is taken 36.7193g, SrCO 30.7079g, BaCO 30.6309g, Li 2cO 30.0294g, Na 2cO 30.0422g, K 2cO 30.055g, Pr 6o 110.4082g, Nb 2o 510.6277g, above raw material is analytical pure, puts into agate mortar and adds after 40g dehydrated alcohol grinds 3 hours, dry in 50 DEG C of baking ovens;
(2) mixed powder after drying to be placed in alumina crucible in air atmosphere at 900 DEG C pre-burning 4 hours;
(3) preburning powdered material after grinding is calcined 4 hours in air atmosphere at 1400 DEG C;
(4) by cooled product physical fragmentation, grinding, ion, oven dry, chemical constitution is namely obtained for (Ca 0.84sr 0.06ba 0.04li 0.01na 0.01k 0.01pr 0.03) 2nb 2o 7lED red fluorescence powder.
The obtained LED of this embodiment is by red fluorescence powder outward appearance in white, and XRD spectra result is basically identical with embodiment 1, and it excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1.
The exciting and launch peak position, calcination atmosphere and temperature and granularity of table 1. embodiment 1-8 sample
The relative luminous intensity (excitation wavelength is 457nm) of embodiment 1-8 sample as shown in Figure 7.Wherein, the relative luminous intensity of embodiment 2-8 sample (x > 0 or y > 0 or x, y > 0) is apparently higher than embodiment 1 sample (x=0, y=0); In embodiment 1-8 sample, the relative luminous intensity of embodiment 6 sample (x=0.04, y=0.02, z=0.02, A=Na) is the highest.
The above; be only explanation embodiment of the present invention; not to any formal and substantial restriction of the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from the inventive method, the some improvement made and supplement also should be considered as protection scope of the present invention.All those skilled in the art, without departing from the spirit and scope of the present invention, a little change utilizing disclosed above technology contents to make, the equivalent variations of modifying and developing, be Equivalent embodiments of the present invention; Meanwhile, all according to substantial technological of the present invention to the change of any equivalent variations that above-described embodiment does, modify and differentiation, all still belong to the scope of technical scheme of the present invention.

Claims (10)

1. a LED red fluorescence powder, it is characterized in that this fluorescent material is the alkaline earth metal niobate fluorescent material that praseodymium activates, its chemical expression is (Ca 1-x-y-2zsr xba ya zpr z) 2nb 2o 7, wherein A represents monovalent base metallic element, is selected from least one in Li, Na, K and Rb; 0≤x≤0.2; 0≤y≤0.1; 0 < z < 0.1.
2. LED red fluorescence powder as claimed in claim 1, it is characterized in that, the span of described x is 0≤x≤0.1.
3. LED red fluorescence powder as claimed in claim 1, it is characterized in that, the span of described y is 0≤y≤0.05.
4. LED red fluorescence powder as claimed in claim 1, it is characterized in that, the span of described z is 0.01≤z≤0.05.
5. the LED red fluorescence powder as described in as arbitrary in claim 1-4, it is characterized in that, the UV-light wave band of excitation wavelength range at 200 ~ 400nm of described LED red fluorescence powder and the blue wave band of 430 ~ 510nm, wherein, the excitation peak of UV-light wave band is positioned at 311nm, and the excitation peak of blue wave band is positioned at 457nm, 476nm and 493nm; Emission wavelength ranges is at 590 ~ 650nm, and emission peak is positioned at 614nm.
6. the preparation method of the LED red fluorescence powder as described in as arbitrary in claim 1-5, is characterized in that comprising the following steps:
1) measure than the raw materials of compound taken containing Elements C a, Sr, Ba, Pr, Nb and A by element chemistry, add deionized water or dehydrated alcohol grinding, mix, dry in 50 ~ 100 DEG C of baking ovens and obtain mixed powder;
2) by step 1) mixed powder pre-burning at 800 ~ 1000 DEG C in air or oxygen of gained, pre-burning soaking time is 1 ~ 5 hour;
3), after being ground by cooled pre-burning product, calcine at 1200 ~ 1450 DEG C in air or oxygen, the sintering soak time is 2 ~ 10 hours;
4) by step 3) carry out after the cooling of the calcinate that obtains pulverizing, grind, clean removal of impurities, oven dry, namely obtain LED red fluorescence powder.
7. preparation method as claimed in claim 6, it is characterized in that, step 1) in, the described raw materials of compound containing Elements C a, Sr, Ba, Pr, Nb and A is selected from the oxide compound of Ca, Sr, Ba, Pr, Nb and A, oxyhydroxide, carbonate, nitrate, oxalate, acetate.
8. preparation method as claimed in claim 6, is characterized in that, step 1) in, during described grinding, the mass ratio of deionized water or dehydrated alcohol and raw mixture is 1: 1 ~ 3: 1, and milling time is 1 ~ 10 hour.
9. preparation method as claimed in claim 6, is characterized in that, step 4) in, described pulverizing can adopt physics fragmentation or comminution by gas stream, and described cleaning comprises one or more in washing, pickling or alkali cleaning.
10. preparation method as claimed in claim 6, is characterized in that, the mean particle size of obtained LED red fluorescence powder is 0.1 ~ 30 μm.
CN201410183921.6A 2014-05-05 2014-05-05 A kind of LED red fluorescence powder and preparation method thereof Expired - Fee Related CN103992795B (en)

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