CN103450898A - Titanate base red fluorescent powder for white LED (Light Emitting Diode) and preparation method thereof - Google Patents
Titanate base red fluorescent powder for white LED (Light Emitting Diode) and preparation method thereof Download PDFInfo
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- CN103450898A CN103450898A CN2013103601797A CN201310360179A CN103450898A CN 103450898 A CN103450898 A CN 103450898A CN 2013103601797 A CN2013103601797 A CN 2013103601797A CN 201310360179 A CN201310360179 A CN 201310360179A CN 103450898 A CN103450898 A CN 103450898A
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Abstract
The invention discloses titanate base red fluorescent powder for a white LED (Light Emitting Diode) and a preparation method thereof. The chemical general formula of the titanate base red fluorescent powder is NaA1-xTiO4:xEu, wherein A is La<3+> or Y<3+>, and x is greater than or equal to 0.001 and is less than or equal to 0.50. The method has high operability and a simple synthesis process and is suitable for large-scale industrial production. The prepared titanate base red fluorescent powder for the white LED has the characteristics of high brightness and high stability, is suitable for ultraviolet, near ultraviolet and blue excitation and meets the operating requirements of the red fluorescent powder for the white LED; the emission intensity and the luminous intensity of the titanate base red fluorescent powder are high, the light mainly comprises red light, the color coordinates of the titanate base red fluorescent powder are that x is equal to 0.664 and y is equal to 0.335; the titanate base red fluorescent powder can be effectively excited by ultraviolet light of 350-400 nm and blue light of 450-470 nm respectively; the red light with wavelength range of 590-650 nm can be excited; the titanate base red fluorescent powder is a superior red fluorescent powder for the LED.
Description
Technical field
The invention belongs to rare earth luminescent material technical field, be specifically related to titanate base red fluorescent powder and preparation method thereof for a kind of white light LEDs.
Background technology
White light LEDs is a kind of efficient, energy-saving and environmental protection, green lighting source, is widely used in various illuminations and demonstration field.
Since the white light LEDs excited with high brightness InGaN blue chip makes a breakthrough technically, white light LEDs is developed rapidly at electron device and lighting field.Japanese Ya chemical company in 1996 takes the lead in succeeding in developing with the InGaN blue chip and coordinates gold-tinted fluorescent material YAG(yttrium aluminum garnet) white LED light source, its chemical formula is Y
3al
5o
12: Ce
3+(U.S. Pat 2008116422-A1).But the design of this white light emission system exists very large defect, due to ruddiness composition deficiency in its utilizing emitted light, and along with the increase of duration of service, chip is aging causes the luminous blue shift that occurs, the mixed light that finally makes this system send is partially blue, and color developing is not high.Therefore research and development can be very urgent tasks by ultraviolet and blue-light excited high brightness, the red fluorescence powder of stable performance, and the universal and development of white light LEDs is had very important significance.
At present, the red fluorescence powder of commercialization mainly contains Y
2o
2s: Eu
3+, Y
2o
3: Eu
3+, (Ca, Sr) S: Eu
2+, (Y, Gd) BO
3: Eu
3+, YVO
4: Eu
3+.But above-mentioned red fluorescence powder ubiquity luminous efficiency is low, poor stability, the easy problem such as aging, and the fluorescent material that can effectively be excited by near ultraviolet and blue light is less, especially the shortage of efficient stable red fluorescence powder, restricted further developing of white light LEDs performance.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, titanate base red fluorescent powder and preparation method thereof for a kind of white light LEDs is provided, its luminous intensity is high, stability is strong.
For achieving the above object, the present invention adopts following technical scheme:
A kind of white light LEDs titanate base red fluorescent powder, the chemical general formula of this titanate base red fluorescent powder is NaA
1-xtiO
4: xEu, wherein, A is La
3+or Y
3+, 0.001≤x≤0.50.
The preparation method of titanate base red fluorescent powder for above-mentioned white light LEDs comprises the following steps:
(1) press chemical general formula NaA
1-xtiO
4: the stoichiometric ratio of xEu, will contain the solid chemical compound of Na element, the solid chemical compound that contains the A element, the solid chemical compound that contains the Ti element, the solid chemical compound that contains the Eu element and fusing assistant and mix, then ground and mixed is even, obtains mixture;
(2) mixture is packed in crucible, and crucible is put into to high-temperature electric resistance furnace and calcine, obtain calcined material;
(3) calcined material pulverized, grind, sieve, washed, drying, obtain white light LEDs titanate base red fluorescent powder.
Fusing assistant in described step (1) is Na
2cO
3, the fusing assistant consumption is 20%～50% of the solid chemical compound amount of substance that contains the Na element.
The solid chemical compound that contains the Na element in described step (1) is Na
2cO
3, the solid chemical compound that contains the Ti element is TiO
2, the solid chemical compound that contains the Eu element is respectively Eu
2o
3, containing the solid chemical compound of A element, be La
2o
3or Y
2o
3.
In described step (1), milling time is 30～60 minutes.
The calcinating system that calcining adopts in described step (2) is, rises to 900～1100 ℃ from room temperature with the temperature rise rate of 10 ℃/min under air atmosphere, and is incubated 2～8 hours.
Sieve and be specially 100 mesh sieves in described step (3); One or both in the concrete employing of washing pickling, washing, wherein, pickling adopts the dilute hydrochloric acid that the pH value is 1 to carry out.
Temperature dry in described step (3) is 120～150 ℃, and the time is 4～8 hours.
With respect to prior art, the beneficial effect that the present invention has: the invention provides a kind of method of white light LEDs with the titanate base red fluorescent powder that prepare, the method is workable, and synthesis technique is simple, is suitable for large-scale industrial production.Because titanate has good thermostability and chemical stability, it is a kind of good luminous host material; Trivalent rare earth ions has abundant energy level, the luminescent material of its doping has broad application prospects in fields such as green illumination, bioluminescence sign, short wavelength laser, information demonstration and photoelectronics, so the present invention adopts white light LEDs prepared by the titanate doping with rare-earth ions to have high brightness with the titanate base fluorescent powder, the characteristics of high stability, be applicable to ultraviolet, near ultraviolet, blue-light excited, meet the service requirements of red fluorescent powder for white radiation LED; Its emission luminous intensity is high, take ruddiness as main, its chromaticity coordinates is: x=0.664, y=0.335, can effectively be excited by the blue light of the UV-light of 350～400nm and 450～470nm respectively, launch the ruddiness that wavelength region is 590～650nm, meet the service requirements of red fluorescent powder for white radiation LED, be the good LED red fluorescence powder of a kind of luminescent properties, there is the market potential using value.Titanate base fluorescent powder and commercial red fluorescence powder Y for white light LEDs prepared by the present invention
2o
2s: Eu
3+compare, not only luminous intensity is high, and its CIE value more approaches desirable ruddiness NTSC(National Television Standard Committee) standard value (x=0.67, y=0.33).
The accompanying drawing explanation
Fig. 1 is the NaLa of embodiment 1 preparation
0.95eu
0.05tiO
4the X-ray diffracting spectrum of red fluorescence powder and NaLaTiO
4standard card (PDF#86-0828) contrast figure.
Fig. 2 is the prepared NaLa of embodiment 2
0.90eu
0.10tiO
4the excitation spectrum of red fluorescence powder and emmission spectrum.
Fig. 3 is the prepared NaLa of embodiment 3
0.85eu
0.15tiO
4the CIE chromaticity coordinates figure of red fluorescence powder.
Fig. 4 is the prepared NaY of embodiment 4
0.95eu
0.05tiO
4the scanning electron microscope (SEM) photograph of red fluorescence powder.
Embodiment
White light LEDs prepared by the present invention titanate base red fluorescent powder, the chemical general formula of this titanate base red fluorescent powder is NaA
1-xtiO
4: xEu, wherein, A is La
3+or Y
3+, 0.001≤x≤0.50.
The preparation method of titanate base red fluorescent powder for white light LEDs of the present invention comprises the following steps:
(1) press chemical general formula NaA
1-xtiO
4: the stoichiometric ratio of xEu, will contain the solid chemical compound of Na element, the solid chemical compound that contains the A element, the solid chemical compound that contains the Ti element, the solid chemical compound that contains the Eu element and fusing assistant and mix, then ground and mixed is even, obtains mixture;
(2) mixture is packed in crucible, and crucible is put into to high-temperature electric resistance furnace and calcine, obtain calcined material;
(3) calcined material pulverized, grind, sieve, washed, drying, obtain white light LEDs titanate base red fluorescent powder.
Fusing assistant in above-mentioned steps (1) is Na
2cO
3, the fusing assistant consumption is 20%～50% of the solid chemical compound amount of substance that contains the Na element.
The solid chemical compound that contains the Na element in above-mentioned steps (1) is Na
2cO
3, the solid chemical compound that contains the Ti element is TiO
2, the solid chemical compound that contains the Eu element is respectively Eu
2o
3, containing the solid chemical compound of A element, be La
2o
3or Y
2o
3.
In above-mentioned steps (1), milling time is 30～60 minutes.
The calcinating system that calcining adopts in above-mentioned steps (2) is, rises to 900～1100 ℃ from room temperature with the temperature rise rate of 10 ℃/min under air atmosphere, and is incubated 2～8 hours.
Sieve and be specially 100 mesh sieves in above-mentioned steps (3); One or both in the concrete employing of washing pickling, washing, wherein, pickling adopts the dilute hydrochloric acid that the pH value is 1 to carry out.
Temperature dry in above-mentioned steps (3) is 120～150 ℃, and the time is 4～8 hours.
Below in conjunction with drawings and Examples, the present invention is described in more detail.
Embodiment 1
A kind of white light LEDs titanate base red fluorescent powder, chemical formula is NaLa
0.95eu
0.05tiO
4.
The preparation method of above-mentioned titanate base red fluorescent powder comprises the following steps:
(1) with Na
2cO
3, La
2o
3, Eu
2o
3, TiO
2for raw material, press Na: La: Eu: Ti=1.3: the amount of substance ratio of 0.95: 0.05: 1, by Na
2cO
3, La
2o
3, Eu
2o
3, TiO
2grind 30 minutes in agate mortar and fully mix, obtaining mixture; Wherein, Na
2cO
3both as reactant, participate in reaction, played fluxing action as fusing assistant again, as the Na of fusing assistant
2cO
3amount of substance account for the Na that participates in reaction
2cO
3amount of substance 30%;
(2) mixture is packed in corundum crucible, corundum crucible is put into to high-temperature electric resistance furnace, under air atmosphere, from room temperature, with the temperature rise rate of 10 ℃/min, rise to 950 ℃, be incubated 4 hours, then cool to room temperature with the furnace, obtain calcined material;
(3) calcined material is pulverized, ground, and, by the accurate sub-sieve of 100 target, extracting screen underflow, then wash screen underflow with the dilute hydrochloric acid of pH=1, then, after 120 ℃ of dry 8h, obtain titanate base red fluorescent powder NaLa for white light LEDs
0.95eu
0.05tiO
4.
Referring to Fig. 1, can find out the present embodiment gained NaLa processed from Fig. 1
0.95eu
0.05tiO
4the X-ray diffractogram of titanate base red fluorescent powder and NaLaTiO
4standard diagram (PDF#86-0828) matches, and proves that prepared fluorescent material is purer, and it belongs to tetragonal system, and spacer is P4/nmm (129).
Embodiment 2
A kind of white light LEDs titanate base red fluorescent powder, chemical formula is NaLa
0.90eu
0.10tiO
4.
The preparation method of above-mentioned titanate base red fluorescent powder comprises the following steps:
(1) with Na
2cO
3, La
2o
3, Eu
2o
3, TiO
2for raw material, press Na: La: Eu: Ti=1.4: the amount of substance ratio of 0.90: 0.10: 1, by Na
2cO
3, La
2o
3, Eu
2o
3, TiO
2grind 40 minutes in agate mortar and fully mix, obtaining mixture; Wherein, Na
2cO
3both as reactant, participate in reaction, played fluxing action as fusing assistant again, as the Na of fusing assistant
2cO
3amount of substance account for the Na that participates in reaction
2cO
3amount of substance 40%;
(2) mixture is packed in corundum crucible, corundum crucible is put into to the heating high-temperature electric resistance furnace, under air atmosphere, from room temperature, with the temperature rise rate of 10 ℃/min, rise to 950 ℃, be incubated 4 hours, then cool to room temperature with the furnace, obtain calcined material;
(3) calcined material is pulverized and ground, and, by the accurate sub-sieve of 100 target, extracting screen underflow, then wash screen underflow with the dilute hydrochloric acid of pH=1, then, in 130 ℃ of dry 6h, obtain titanate base red fluorescent powder NaLa for white light LEDs
0.90eu
0.10tiO
4.
Referring to Fig. 2, as can be seen from Figure 2, white light LEDs prepared by the present embodiment has carried out excitation spectrum and emmission spectrum test with the titanate base red fluorescent powder.The titanate base red fluorescent powder is launched the ruddiness of 619nm under the exciting of the near-ultraviolet light of 396nm, and excitation wavelength and near ultraviolet GaN chip are complementary, and illustrates that this fluorescent material can be used as the red composition of near ultraviolet excitation white light LEDs.
Embodiment 3
A kind of white light LEDs titanate base red fluorescent powder, chemical formula is NaLa
0.85eu
0.15tiO
4.
The preparation method of above-mentioned titanate base red fluorescent powder comprises the following steps:
(1) press NaLa
0.85eu
0.15tiO
4stoichiometric ratio, press Na: La: Eu: Ti=1.5: the amount of substance ratio of 0.85: 0.15: 1, by Na
2cO
3, La
2o
3, Eu
2o
3, TiO
2grind 50 minutes in agate mortar and fully mix, obtaining mixture; Wherein, Na
2cO
3both as reactant, participate in reaction, played fluxing action as fusing assistant again, as the Na of fusing assistant
2cO
3amount of substance account for the Na that participates in reaction
2cO
3amount of substance 50%;
(2) mixture is packed in corundum crucible, corundum crucible is put into to high-temperature electric resistance furnace, under air atmosphere, from room temperature, with the temperature rise rate of 10 ℃/min, rise to 900 ℃, be incubated 6 hours, then cool to room temperature with the furnace, obtain calcined material;
(3) calcined material is pulverized, ground, by the accurate sub-sieve of 100 target, extracting screen underflow, then wash screen underflow with the dilute hydrochloric acid of pH=1, then, in 140 ℃ of dry 5h, obtain titanate base red fluorescent powder NaLa for white light LEDs
0.85eu
0.15tiO
4.
Referring to Fig. 3, as can be seen from Figure 3, the prepared NaLa of the present embodiment
0.85eu
0.15tiO
4chromaticity coordinates be: x=0.664, y=0.335.Titanate base fluorescent powder and commercial red fluorescence powder Y for white light LEDs prepared by the present invention
2o
2s: Eu
3+compare, not only luminous intensity is high, and its CIE value more approaches desirable ruddiness NTSC(National Television Standard Committee) standard value (x=0.67, y=0.33).
Embodiment 4
A kind of white light LEDs titanate base red fluorescent powder, chemical formula is NaY
0.95eu
0.05tiO
4.
The preparation method of above-mentioned titanate base red fluorescent powder comprises the following steps:
(1) press NaY
0.95eu
0.05tiO
4stoichiometric ratio, press Na: Y: Eu: Ti=1.3: the ratio of the amount of substance of 0.95: 0.05: 1.By Na
2cO
3, Y
2o
3, Eu
2o
3, TiO
2grind 60 minutes in agate mortar and fully mix, obtaining mixture; Wherein, Na
2cO
3both as reactant, participate in reaction, played fluxing action as fusing assistant again, as the Na of fusing assistant
2cO
3amount of substance account for the Na that participates in reaction
2cO
3amount of substance 30%;
(2) mixture is packed in corundum crucible, corundum crucible is put into to high-temperature electric resistance furnace, under air atmosphere, from room temperature, with the temperature rise rate of 10 ℃/min, rise to 1050 ℃, be incubated 4 hours, then cool to room temperature with the furnace, obtain calcined material;
(3) calcined material is pulverized, ground, and, by the accurate sub-sieve of 100 target, extracting screen underflow, then wash screen underflow with the dilute hydrochloric acid of pH=1, and, in 140 ℃ of dry 5h, obtain red fluorescence powder NaY
0.95eu
0.05tiO
4.
Referring to Fig. 4, as can be seen from Figure 4, NaY prepared by the present embodiment
0.95eu
0.05tiO
4the fluorescent material grain-size is 2～5 μ m, and its pattern rule, approaches cubic shape, and this proves mutually with X-ray diffracting spectrum.
Embodiment 5
A kind of white light LEDs titanate base red fluorescent powder, chemical formula is NaY
0.90eu
0.10tiO
4.
The preparation method of above-mentioned titanate base red fluorescent powder comprises the following steps:
(1) press NaY
0.90eu
0.10tiO
4stoichiometric ratio, press Na: Y: Eu: Ti=1.4: the amount of substance ratio of 0.90: 0.10: 1, by Na
2cO
3, Y
2o
3, Eu
2o
3, TiO
2grind 30 minutes in agate mortar and fully mix, obtaining mixture; Wherein, Na
2cO
3both as reactant, participate in reaction, played fluxing action as fusing assistant again, as the Na of fusing assistant
2cO
3amount of substance account for the Na that participates in reaction
2cO
3amount of substance 40%;
(2) mixture is packed in corundum crucible, corundum crucible is put into to high-temperature electric resistance furnace, under air atmosphere, from room temperature, with the temperature rise rate of 10 ℃/min, rise to 1050 ℃, be incubated 4 hours, then cool to room temperature with the furnace, obtain calcined material;
(3) calcined material is ground gained fluorescent material, also pass through the accurate sub-sieve of 100 target, extracting screen underflow, then wash screen underflow with the dilute hydrochloric acid of pH=1, then, in 120 ℃ of dry 8h, obtain red fluorescence powder NaY
0.90eu
0.10tiO
4.
Embodiment 6
A kind of white light LEDs titanate base red fluorescent powder, chemical formula is NaLa
0.999eu
0.001tiO
4.
The preparation method of above-mentioned titanate base red fluorescent powder comprises the following steps:
(1) press NaLa
0.999eu
0.001tiO
4stoichiometric ratio, press Na: La: Eu: Ti=1.2: the amount of substance ratio of 0.999: 0.001: 1, by Na
2cO
3, La
2o
3, Eu
2o
3, TiO
2grind 35 minutes in agate mortar and fully mix, obtaining mixture; Wherein, Na
2cO
3both as reactant, participate in reaction, played fluxing action as fusing assistant again, as the Na of fusing assistant
2cO
3amount of substance account for the Na that participates in reaction
2cO
3amount of substance 20%;
(2) mixture is packed in corundum crucible, corundum crucible is put into to high-temperature electric resistance furnace, under air atmosphere, from room temperature, with the temperature rise rate of 10 ℃/min, rise to 1100 ℃, be incubated 2 hours, then cool to room temperature with the furnace, obtain calcined material;
(3) calcined material is ground gained fluorescent material, and, by the accurate sub-sieve of 100 target, extracting screen underflow, then successively wash screen underflow with dilute hydrochloric acid and the water of pH=1; In 140 ℃ of dry 4h, obtain red fluorescence powder NaLa again
0.999eu
0.001tiO
4.
Embodiment 7
A kind of white light LEDs titanate base red fluorescent powder, chemical formula is NaY
0.994eu
0.006tiO
4.
The preparation method of above-mentioned titanate base red fluorescent powder comprises the following steps:
(1) press NaY
0.994eu
0.006tiO
4stoichiometric ratio, press Na: Y: Eu: Ti=1.25: the amount of substance ratio of 0.994: 0.006: 1, by Na
2cO
3, Y
2o
3, Eu
2o
3, TiO
2grind 45 minutes in agate mortar and fully mix, obtaining mixture; Wherein, Na
2cO
3both as reactant, participate in reaction, played fluxing action as fusing assistant again, as the Na of fusing assistant
2cO
3amount of substance account for the Na that participates in reaction
2cO
3amount of substance 25%;
(2) mixture is packed in corundum crucible, corundum crucible is put into to high-temperature electric resistance furnace, under air atmosphere, from room temperature, with the temperature rise rate of 10 ℃/min, rise to 900 ℃, be incubated 6 hours, then cool to room temperature with the furnace, obtain calcined material;
(3) calcined material is ground gained fluorescent material, also pass through the accurate sub-sieve of 100 target, extracting screen underflow, then wash screen underflow with water, then, in 130 ℃ of dry 6h, obtain red fluorescence powder NaY
0.994eu
0.006tiO
4.
Embodiment 8
A kind of white light LEDs titanate base red fluorescent powder, chemical formula is NaLa
0.8eu
0.2tiO
4.
The preparation method of above-mentioned titanate base red fluorescent powder comprises the following steps:
(1) press NaLa
0.8eu
0.2tiO
4stoichiometric ratio, press Na: La: Eu: Ti=1.35: the amount of substance ratio of 0.8: 0.2: 1, by Na
2cO
3, La
2o
3, Eu
2o
3, TiO
2grind 55 minutes in agate mortar and fully mix, obtaining mixture; Wherein, Na
2cO
3both as reactant, participate in reaction, played fluxing action as fusing assistant again, as the Na of fusing assistant
2cO
3amount of substance account for the Na that participates in reaction
2cO
3amount of substance 35%;
(2) mixture is packed in corundum crucible, corundum crucible is put into to high-temperature electric resistance furnace, under air atmosphere, from room temperature, with the temperature rise rate of 10 ℃/min, rise to 900 ℃, be incubated 8 hours, then cool to room temperature with the furnace, obtain calcined material;
(3) calcined material is ground gained fluorescent material, also pass through the accurate sub-sieve of 100 target, extracting screen underflow, then successively wash screen underflow with dilute hydrochloric acid and the water of pH=1, then, in 120 ℃ of dry 7h, obtain red fluorescence powder NaLa
0.8eu
0.2tiO
4.
Embodiment 9
A kind of white light LEDs titanate base red fluorescent powder, chemical formula is NaY
0.7eu
0.3tiO
4.
The preparation method of above-mentioned titanate base red fluorescent powder comprises the following steps:
(1) press NaY
0.70eu
0.30tiO
4stoichiometric ratio, press Na: Y: Eu: Ti=1.45: the amount of substance ratio of 0.70: 0.30: 1, by Na
2cO
3, Y
2o
3, Eu
2o
3, TiO
2grind 60 minutes in agate mortar and fully mix, obtaining mixture; Wherein, Na
2cO
3both as reactant, participate in reaction, played fluxing action as fusing assistant again, as the Na of fusing assistant
2cO
3amount of substance account for the Na that participates in reaction
2cO
3amount of substance 45%;
(2) mixture is packed in corundum crucible, corundum crucible is put into to high-temperature electric resistance furnace, under air atmosphere, from room temperature, with the temperature rise rate of 10 ℃/min, rise to 1000 ℃, be incubated 4 hours, then cool to room temperature with the furnace, obtain calcined material;
(3) by calcined material by gained fluorescent material grind, and by the accurate sub-sieve of 100 target, extracting screen underflow, then wash screen underflow with water, then under 150 ℃ dry 4h, obtain red fluorescence powder NaY
0.70eu
0.30tiO
4.
Embodiment 10
A kind of white light LEDs titanate base red fluorescent powder, chemical formula is NaY
0.50eu
0.50tiO
4.
The preparation method of above-mentioned titanate base red fluorescent powder comprises the following steps:
(1) press NaY
0.50eu
0.50tiO
4stoichiometric ratio, press Na: Y: Eu: Ti=1.25: the amount of substance ratio of 0.50: 0.50: 1, by Na
2cO
3, Y
2o
3, Eu
2o
3, TiO
2grind 60 minutes in agate mortar and fully mix, obtaining mixture; Wherein, Na
2cO
3both as reactant, participate in reaction, played fluxing action as fusing assistant again, as the Na of fusing assistant
2cO
3amount of substance account for the Na that participates in reaction
2cO
3amount of substance 25%;
(2) mixture is packed in corundum crucible, corundum crucible is put into to high-temperature electric resistance furnace, under air atmosphere, from room temperature, with the temperature rise rate of 10 ℃/min, rise to 900 ℃, be incubated 6 hours, then cool to room temperature with the furnace, obtain calcined material;
(3) calcined material is ground gained fluorescent material, also pass through the accurate sub-sieve of 100 target, extracting screen underflow, then wash screen underflow with the dilute hydrochloric acid of pH=1, then, in 120 ℃ of dry 8h, obtain NaY
0.50eu
0.50tiO
4the titanate base red fluorescent powder.
The excitation wavelength of the titanate base red fluorescent powder that the present invention makes is 350～400nm and 450～470nm, and emission wavelength is 590～650nm, and main emission peak is positioned at 619nm.
Because titanate has good thermostability and chemical stability, it is a kind of good luminous host material; Trivalent rare earth ions has abundant energy level, the luminescent material of its doping has broad application prospects in fields such as green illumination, bioluminescence sign, short wavelength laser, information demonstration and photoelectronics, so the titanate base red fluorescent powder luminescent properties that the present invention makes is perfected, and has the market potential using value.
Claims (8)
1. a white light LEDs titanate base red fluorescent powder, is characterized in that, the chemical general formula of this titanate base red fluorescent powder is NaA
1-xtiO
4: xEu, wherein, A is La
3+or Y
3+, 0.001≤x≤0.50.
2. the preparation method of titanate base red fluorescent powder for a kind of white light LEDs as claimed in claim 1, is characterized in that, comprises the following steps:
(1) press chemical general formula NaA
1-xtiO
4: the stoichiometric ratio of xEu, will contain the solid chemical compound of Na element, the solid chemical compound that contains the A element, the solid chemical compound that contains the Ti element, the solid chemical compound that contains the Eu element and fusing assistant and mix, then ground and mixed is even, obtains mixture;
(2) mixture is packed in crucible, and crucible is put into to high-temperature electric resistance furnace and calcine, obtain calcined material;
(3) calcined material pulverized, grind, sieve, washed, drying, obtain white light LEDs titanate base red fluorescent powder.
3. the preparation method of titanate base red fluorescent powder for a kind of white light LEDs according to claim 2, it is characterized in that: the fusing assistant in described step (1) is Na
2cO
3, the fusing assistant consumption is 20%～50% of the solid chemical compound amount of substance that contains the Na element.
4. the preparation method of titanate base red fluorescent powder for a kind of white light LEDs according to claim 2, it is characterized in that: the solid chemical compound that contains the Na element in described step (1) is Na
2cO
3, the solid chemical compound that contains the Ti element is TiO
2, the solid chemical compound that contains the Eu element is Eu
2o
3, the solid chemical compound that contains the A element is La
2o
3or Y
2o
3.
5. the preparation method of titanate base red fluorescent powder for a kind of white light LEDs according to claim 2, it is characterized in that: in described step (1), milling time is 30～60 minutes.
6. the preparation method of titanate base red fluorescent powder for a kind of white light LEDs according to claim 2, it is characterized in that: the calcinating system that in described step (2), calcining adopts is, rise to 900～1100 ℃ from room temperature with the temperature rise rate of 10 ℃/min under air atmosphere, and be incubated 2～8 hours.
7. the preparation method of titanate base red fluorescent powder for a kind of white light LEDs according to claim 2, is characterized in that: in described step (3), sieve and be specially 100 mesh sieves; One or both during washing is specially and adopts pickling, washes, wherein, pickling adopts the dilute hydrochloric acid that the pH value is 1 to carry out.
8. the preparation method of titanate base red fluorescent powder for a kind of white light LEDs according to claim 2, it is characterized in that: temperature dry in described step (3) is 120～150 ℃, and the time is 4～8 hours.
Priority Applications (1)
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| CN105176525A (en) * | 2013-07-25 | 2015-12-23 | 惠州市西顿工业发展有限公司 | LED lamp and preparation method of red-emitting inorganic luminescent material adopted by same |
| CN108913141A (en) * | 2018-08-01 | 2018-11-30 | 苏州大学张家港工业技术研究院 | Eu3+Ion-activated fluorescent material and its preparation and application |
| CN109762564A (en) * | 2019-03-13 | 2019-05-17 | 常州工程职业技术学院 | A kind of europium ion Eu3+The titanate red fluorescence powder of activation, preparation method and applications |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105176525A (en) * | 2013-07-25 | 2015-12-23 | 惠州市西顿工业发展有限公司 | LED lamp and preparation method of red-emitting inorganic luminescent material adopted by same |
| CN108913141A (en) * | 2018-08-01 | 2018-11-30 | 苏州大学张家港工业技术研究院 | Eu3+Ion-activated fluorescent material and its preparation and application |
| CN108913141B (en) * | 2018-08-01 | 2021-04-20 | 苏州大学张家港工业技术研究院 | Eu3+Ion-activated fluorescent material, preparation and application thereof |
| CN109762564A (en) * | 2019-03-13 | 2019-05-17 | 常州工程职业技术学院 | A kind of europium ion Eu3+The titanate red fluorescence powder of activation, preparation method and applications |
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