CN103992795A - Red phosphor for LED, and preparation method thereof - Google Patents
Red phosphor for LED, and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a red phosphor for LED. The red phosphor is a praseodymium activated alkaline earth metal columbate fluorescence material. The chemical expression formula of the red phosphor is (Ca1xy2zSrxBayAzPrz)2Nb2O7, wherein A represents a monovalent alkali metal element and is selected from at least one of Li, Na, K and Rb; x is not greater than 0.2 and not lower than 0; y is not greater than 0.1 and not lower than 0; and z is not greater than 0.05 and greater than 0. A preparation method of the phosphor through a high temperature solid phase process comprises the following steps: weighing compounds containing corresponding elements according to the stoichiometric ratio of the chemical expression formula, mixing, uniformly grinding, drying, pre-burning and carrying out high temperature calcining in air or oxygen environment, crushing, grinding, cleaning to remove impurities, and drying. The phosphor has the advantages of simple preparation method, no pollution, low cost, wide excitation wavelength range, excellent luminescence performance, high color rendering index, good temperature stability, moisture resistance and the like, and can be widely used in ultraviolet or blue LED chips to make white LED.
Description
Technical field
The present invention relates to alkaline earth metal niobate red fluorescence powder of a kind of praseodymium activation and preparation method thereof, be particularly useful for red fluorescence powder of LED and preparation method thereof, belong 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 of being made by blueness or near ultraviolet LED chip and the combination of light conversion phosphor.This novel solid light source is than 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, there is huge application prospect in illumination and demonstration field, be expected to realize industrialization, substitute existing lighting fixtures, become the 4th generation lighting source.
Adopt LED chip and phosphor combination to produce white light and have three kinds of modes: blue led chip and yellow fluorescent powder combination; Blue led chip and red, green emitting phosphor combination; Near ultraviolet or purple LED chip and the combination of red, green, blue three primary colors fluorescent powder.Adopt at present blue light GaN or InGaN base LED chip to apply yellow fluorescent powder Y
3al
5o
12: Ce
3+(YAG:Ce) high-brightness white-light LED of making has been realized commercialization, and has entered special lighting field.But there is because lacking red spectral band transmitting the inherent defect that colour rendering index is lower 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 colour temperature thereof any coupling within the scope of 2500~10000K.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, easy deliquescence need be coated processing when 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 and there is the more red fluorescent powder for white radiation LED of premium properties.The calcium niobate of doped with rare-earth elements itself is not a kind of piezoelectricity, photoelectricity, ferroelectric material of high-quality, has good moistureproofness, thermostability and chemical stability.The present invention is the requirement that adapts to white light LEDs technical development, has developed alkaline earth metal niobate red fluorescence powder of a kind of activation of the praseodymium for white light LEDs and preparation method thereof.
Summary of the invention
The object of the present invention is to provide one to be excited by UV-light or blue-ray LED, there is good luminous characteristic and physicochemical characteristic, and red fluorescence powder and preparation method thereof for the LED that preparation method is simple, pollution-free, cost is low, to overcome problems of the prior art.
To achieve these goals, the present invention realizes by the following technical solutions:
LED of the present invention is the alkaline earth metal niobate fluorescent material that praseodymium activates with red fluorescence powder, 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, does not mate for the electric charge compensating after the alternative divalent alkaline-earth metal ion of trivalent rare earth praseodymium ion, thereby reaches minimizing fault in material, improves the object of luminous intensity.
The preparation method of red fluorescence powder for LED of the present invention, comprises following processing step:
(1) measure than the raw materials of compound taking containing Elements C a, Sr, Ba, Pr, Nb and A by element chemistry, add deionized water or dehydrated alcohol to grind, mix, in 50~100 DEG C of baking ovens, dry and obtain mixed powder;
(2) by mixed powder pre-burning at 800~1000 DEG C in air or oxygen of step (1) gained, pre-burning soaking time is 1~5 hour;
(3) after cooled pre-burning product is ground, calcining at 1200~1450 DEG C in air or oxygen, calcining soaking time is 2~10 hours;
(4) after the calcinate that step (3) obtained is cooling, pulverize, grind, clean removal of impurities, oven dry, 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 oxide compound, oxyhydroxide, carbonate, nitrate, oxalate, the acetate of Ca, Sr, Ba, Pr, Nb and A.
In above-mentioned steps (1), when 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 physics fragmentation or comminution by gas stream, cleans one or more that comprise in washing, pickling or alkali cleaning.
In above-mentioned steps (4), the LED making is 0.1~30 μ m by the mean particle size of red fluorescence powder.
Feature of the present invention is:
(1) LED the present invention relates to is simple, pollution-free with red fluorescence powder, preparation method thereof, cost is low.
(2) the LED red light emitting phosphor excellent property that the present invention makes, has higher colour rendering index, and the temperature stability under room temperature to 300 DEG C condition is good, and physicochemical property are stable, water-fast protection against the tide.
(3) LED that the present invention makes is wide by red fluorescence powder excitation wavelength range, 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 chip emmission spectrum scope is at 430~500nm, and emission peak is positioned at 460 ± 10nm, fully mates with the excitation peak of red fluorescence powder blue wave band with LED of the present invention.LED of the present invention is with the emission peak wavelength of red fluorescence powder at 590~650nm, and transmitting main peak is positioned at 614nm, can make up well and in current white light LEDs, lack red spectral band or the weak deficiency of red spectral band transmitting.
(4) the LED red fluorescence powder that the present invention makes, can combine with green emitting phosphor, is coated on blue led chip, prepares white light LEDs; Or coordinate the preparation as red fluorescence part for white light LEDs with ultraviolet leds; Also or with UV-light, blue-ray LED coordinate, with other color phosphor combination, prepare the different color LED of color.
Brief description of the drawings
Fig. 1 is Ca
2nb
2o
7powdery diffractometry standard card (18-0301) and embodiment 1 sample (Ca
098k
001pr
001)
2nb
2o
7x ray powder diffraction pattern.
Fig. 2 is monitoring embodiment 1 sample (Ca
098k
001pr
001)
2nb
2o
7the exciting light spectrogram of 614nm red emission.
Fig. 3 is 311nm ultraviolet excitation embodiment 1 sample (Ca
098k
0.01pr
001)
2nb
2o
7the utilizing emitted light spectrogram obtaining.
Fig. 4 is the blue-light excited embodiment 1 sample (Ca of 457nm
098k
001pr
001)
2nb
2o
7the utilizing emitted light spectrogram obtaining.
Fig. 5 is the blue-light excited embodiment 1 sample (Ca of 476nm
098k
001pr
001)
2nb
2o
7the utilizing emitted light spectrogram obtaining.
Fig. 6 is the blue-light excited embodiment 1 sample (Ca of 493nm
098k
001pr
001)
2nb
2o
7the utilizing emitted light spectrogram obtaining.
Fig. 7 is the comparison diagram of the relative luminous intensity (excitation wavelength is 457nm) of embodiment 1-8 sample.
specific embodiments
Below by 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 before and after described combination step also there is other method steps, or can also insert other method steps before the step of clearly mentioning at these; Should also be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.And, except as otherwise noted, the numbering of various method steps is only for differentiating the convenient tool of various method steps, but not for limiting the ordering of various method steps or limiting the enforceable scope of the present invention, the change of its relativeness or adjustment, in the situation that changing technology contents without essence, when being also considered as the enforceable category of the present invention.
Embodiment 1
(Ca
098k
001pr
001)
2nb
2o
7the preparation of sample:
(1) take raw materials of Ca CO
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 30g dehydrated alcohol to grind after 2 hours, in 60 DEG C of baking ovens, dries;
(2) mixed powder after drying is placed in alumina crucible in air atmosphere at 900 DEG C to pre-burning 4 hours;
(3) preburning powdered material after grinding is calcined 4 hours in air atmosphere at 1400 DEG C;
(4), by the fragmentation of cooled product physics, grinding, washing removal of impurities, oven dry, obtain chemical constitution for (Ca
098k
001pr
001)
2nb
2o
7lED red fluorescence powder.
The LED that this embodiment prepares is white in color by red fluorescence powder outward appearance, and X-ray powder diffraction (XRD) is tested and shown, as shown in Figure 1, and diffraction peak data and the Ca of gained sample
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 that excitation peak is positioned at 200~400nm UV-light wave band of 311nm and excitation peak and is positioned at 430~510nm blue wave band of 457nm, 476nm and 493nm.Current mature InGaN blue led chip 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 has provided respectively the LED emmission spectrum of red fluorescence powder under 311nm UV-light, 457nm blue light, 476nm blue light and 493nm are blue-light excited that this embodiment prepares.As seen from the figure, the emission wavelength ranges of this fluorescent material is at 590~650nm, and transmitting main peak is at 614nm, can make up well and in current white light LEDs, lack red spectral band or the weak deficiency of red spectral band transmitting.The LED that this embodiment makes excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1 with red fluorescence powder.
Embodiment 2
(Ca
097na
0015pr
0015)
2nb
2o
7the preparation of sample:
(1) take raw materials of Ca CO
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 25g dehydrated alcohol to grind after 1.5 hours, in 70 DEG C of baking ovens, dries;
(2) mixed powder after drying is placed in alumina crucible in air atmosphere at 850 DEG C to pre-burning 4 hours;
(3) preburning powdered material after grinding is calcined 6 hours in air atmosphere at 1350 DEG C;
(4), by the fragmentation of cooled product physics, grinding, washing removal of impurities, oven dry, obtain chemical constitution for (Ca
097na
0015pr
0015)
2nb
2o
7lED red fluorescence powder.
The LED that this embodiment makes is white in color by red fluorescence powder outward appearance, and XRD spectra result and embodiment 1 are basically identical, and it excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1.
Embodiment 3
(Ca
0938r
005k
001pr
001)
2nb
2o
7the preparation of sample:
(1) take raw materials of Ca CO
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 35g deionized water to grind after 2.5 hours, in 80 DEG C of baking ovens, dries;
(2) mixed powder after drying is placed in alumina crucible in air atmosphere at 850 DEG C to pre-burning 5 hours;
(3) preburning powdered material after grinding is calcined 8 hours in oxygen atmosphere at 1350 DEG C;
(4), by the fragmentation of cooled product physics, grinding, washing removal of impurities, oven dry, obtain chemical constitution for (Ca
093sr
005k
001pr
001)
2nb
2o
7lED red fluorescence powder.
The LED that this embodiment makes is white in color by red fluorescence powder outward appearance, and XRD spectra result and embodiment 1 are basically identical, and it excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1.
Embodiment 4
(Ca
093ba
005li
001pr
001)
2nb
2o
7the preparation of sample:
(1) take raw materials of Ca CO
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 20g dehydrated alcohol to grind after 2 hours, in 50 DEG C of baking ovens, dries;
(2) mixed powder after drying is placed in alumina crucible in air atmosphere at 900 DEG C to pre-burning 4 hours;
(3) preburning powdered material after grinding is calcined 5 hours in oxygen atmosphere at 1380 DEG C;
(4), by the fragmentation of cooled product physics, grinding, washing removal of impurities, oven dry, obtain chemical constitution for (Ca
093ba
005li
001pr
001)
2nb
2o
7lED red fluorescence powder.
The LED that this embodiment makes is white in color by red fluorescence powder outward appearance, and XRD spectra result and embodiment 1 are basically identical, and it excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1.
Embodiment 5
(Ca
086sr
01na
001k
001pr
002)
2nb
2o
7the preparation of sample:
(1) take raw materials of Ca CO
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 20g deionized water to grind after 1.5 hours, in 80 DEG C of baking ovens, dries;
(2) mixed powder after drying is placed in alumina crucible in air atmosphere at 850 DEG C to pre-burning 5 hours;
(3) preburning powdered material after grinding is calcined 8 hours in oxygen atmosphere at 1300 DEG C;
(4), by the fragmentation of cooled product physics, grinding, washing removal of impurities, oven dry, obtain chemical constitution for (Ca
086sr
01na
001k
001pr
002)
2nb
2o
7lED red fluorescence powder.
The LED that this embodiment makes is white in color by red fluorescence powder outward appearance, and XRD spectra result and embodiment 1 are basically identical, and it excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1.
Embodiment 6
(Ca
09sr
004ba
002na
002pr
002)
2nb
2o
7the preparation of sample:
(1) take raw materials of Ca CO
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 40g deionized water to grind after 3 hours, in 80 DEG C of baking ovens, dries;
(2) mixed powder after drying is placed in alumina crucible in oxygen atmosphere at 900 DEG C to pre-burning 6 hours;
(3) preburning powdered material after grinding is calcined 8 hours in oxygen atmosphere at 1350 DEG C;
(4), by the fragmentation of cooled product physics, grinding, washing removal of impurities, oven dry, obtain chemical constitution for (Ca
09sr
0.04ba
002na
002pr
002)
2nb
2o
7lED red fluorescence powder.
The LED that this embodiment makes is white in color by red fluorescence powder outward appearance, and XRD spectra result and embodiment 1 are basically identical, and it excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1.
Embodiment 7
(Ca
0868r
005ba
005na
001k
001pr
002)
2nb
2o
7the preparation of sample:
(1) take raw materials of Ca CO
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 40g dehydrated alcohol to grind after 3 hours, in 50 DEG C of baking ovens, dries;
(2) mixed powder after drying is placed in alumina crucible in oxygen atmosphere at 850 DEG C to pre-burning 5 hours;
(3) preburning powdered material after grinding is calcined 5 hours in oxygen atmosphere at 1390 DEG C;
(4), by the fragmentation of cooled product physics, grinding, washing removal of impurities, oven dry, obtain chemical constitution for (Ca
086sr
005ba
0.05na
001k
001pr
002)
2nb
2o
7lED red fluorescence powder.
The LED that this embodiment makes is white in color by red fluorescence powder outward appearance, and XRD spectra result and embodiment 1 are basically identical, and it excites peak position, transmitting peak position, calcination atmosphere, calcining temperature, granularity data as shown in table 1.
Embodiment 8
(Ca
084sr
006ba
004li
001na
001k
001pr
003)
2nb
2o
7the preparation of sample:
(1) take raw materials of Ca CO
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 40g dehydrated alcohol to grind after 3 hours, in 50 DEG C of baking ovens, dries;
(2) mixed powder after drying is placed in alumina crucible in air atmosphere at 900 DEG C to pre-burning 4 hours;
(3) preburning powdered material after grinding is calcined 4 hours in air atmosphere at 1400 DEG C;
(4), by the fragmentation of cooled product physics, grinding, washing removal of impurities, oven dry, obtain chemical constitution for (Ca
084sr
006ba
004li
001na
001k
001pr
003)
2nb
2o
7lED red fluorescence powder.
The LED that this embodiment makes is white in color by red fluorescence powder outward appearance, and XRD spectra result and embodiment 1 are basically identical,
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 samples (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; do not departing under the prerequisite of the inventive method some improvement of making and the supplementary protection scope of the present invention that also should be considered as.All those skilled in the art, without departing from the spirit and scope of the present invention, utilize a little change that disclosed above technology contents makes, modify and the equivalent variations of differentiation, are equivalent embodiment of the present invention; , the change of any equivalent variations that all foundations essence technology of the present invention is done above-described embodiment, modify and differentiation meanwhile, all still belong to the scope of technical scheme of the present invention.
Claims (10)
1. a LED red fluorescence powder, is characterized in that this fluorescent material 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.
2. LED red fluorescence powder as claimed in claim 1, is characterized in that, the span of described x is 0≤x≤0.1.
3. LED red fluorescence powder as claimed in claim 1, is characterized in that, the span of described x is 0≤y≤0.05.
4. LED red fluorescence powder as claimed in claim 1, is characterized in that, the span of described x is 0.01≤z≤0.05.
5. the LED red fluorescence powder as described in claim 1-4, it is characterized in that, described LED uses the excitation wavelength range of red fluorescence powder at 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; Emission wavelength ranges is at 590~650nm, and emission peak is positioned at 614nm.
6. the preparation method of red fluorescence powder for the LED 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 taking containing Elements C a, Sr, Ba, Pr, Nb and A by element chemistry, add deionized water or dehydrated alcohol to grind, mix, in 50~100 DEG C of baking ovens, dry 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 cooled pre-burning product is ground, calcining at 1200~1450 DEG C in air or oxygen, calcining soaking time is 2~10 hours;
4) by step 3) pulverize, grind, clean removal of impurities, oven dry after the calcinate that obtains is cooling, 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 oxide compound, oxyhydroxide, carbonate, nitrate, oxalate, the acetate of Ca, Sr, Ba, Pr, Nb and A.
8. preparation method as claimed in claim 6, is characterized in that step 1) in, when described grinding, the mass ratio of deionized water or dehydrated alcohol and raw mixture is 1: 1~3: 1, 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 LED making is 0.1~30 μ m by the mean particle size of red fluorescence powder.
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CN105885833A (en) * | 2016-04-06 | 2016-08-24 | 青岛大学 | Single-component white-light-emitting phosphor and preparation method thereof |
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CN105542765A (en) * | 2015-11-30 | 2016-05-04 | 青岛大学 | Columbate red high brightness elastic stress luminescent material and preparation method thereof |
CN105694884A (en) * | 2016-04-06 | 2016-06-22 | 青岛大学 | Fluorescent powder with lighting color controlled by preparation method and application of fluorescent powder |
CN105885833A (en) * | 2016-04-06 | 2016-08-24 | 青岛大学 | Single-component white-light-emitting phosphor and preparation method thereof |
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