CN102382650A - Nitride red phosphor synthesized at normal pressure for white light and backlight LED - Google Patents
Nitride red phosphor synthesized at normal pressure for white light and backlight LED Download PDFInfo
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- CN102382650A CN102382650A CN201010269713XA CN201010269713A CN102382650A CN 102382650 A CN102382650 A CN 102382650A CN 201010269713X A CN201010269713X A CN 201010269713XA CN 201010269713 A CN201010269713 A CN 201010269713A CN 102382650 A CN102382650 A CN 102382650A
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Abstract
The invention provides nitride red phosphor synthesized at normal pressure for white light and backlight LED. The molecular formula of the nitride red phosphor is A1-xBxEuyAlSiN3, wherein, x is in a range of 0.0 to 0.5, y is in a range of 0.001 to 0.2, and B is one or more selected from the group consisting of Ca, Sr and Ba. The invention is characterized in that: the method comprises the steps of adding 1.90 to 1.999 mol of A, 0.001 to 0.2 mol of EuX3 (x=F, Cl, Br, I, O) and 0.333 mol of Si3N4 into 0.01 to 0.10 mol of the cosolvent NH4X (X=F, Cl), fully mixing 1 mol of AlN to obtain a mixture, calcining the mixture in nitrogen for 3 to 15 hours at a temperature of 1300 to 2000 DEG C, cooling the mixture to room temperature, taking the mixture out for ball milling and rinsing, drying an obtained product for 5 to 12 hours at a temperature of 120 DEG C and sieving the product with a 200-mesh screen.
Description
Technical field
The invention belongs to rare earth luminous and the semiconductor solid lighting field.Relate to the rare earth luminescent material that synthetic white light and backlight are used under a kind of normal pressure, especially a kind of red fluorescence powder of nitride
Background technology
Along with the led chip technology rapid development, it relies on the life-span of LED overlength and high luminous efficiency, and LED shows that in illumination and backlight the field is improved rapidly.Realize the LED lighting field, need obtain the lighting source of white light LEDs and high-color rendering efficiently.Gold-tinted and yellow light mix are all used in the LED encapsulation of using at present, owing to lack ruddiness, its color developing is very low, has had a strong impact on the quality of illuminating ray.Simultaneously present display backlight makes images displayed lose genuine phenomenon because the colour gamut that the chromaticity coordinates of red composition is formed is narrower.USP 6252254 has been reported several kinds of sulfide rouge and powder patents, through manage the better but stable extreme difference of luminosity, encapsulates the elegant and brightness of thick generation chromaticity coordinates and seriously decays.Document Electrochemical and Solid-State Letters, 9,4; H22-H25, the nitride red fluorescent powder of 2006 reports need use 10 normal atmosphere more than 1600 degree, could synthesize equipment requirements; High operation is difficult for, and raw material use metal europium, and is very unstable.Therefore the red fluorescence powder that exploitation can the synthetic efficient stable under normal pressure is necessary.
Summary of the invention
In order to overcome above-mentioned shortcoming.Synthetic white light and backlight LED are used nitride red fluorescent powder under a kind of normal pressure, and its molecular formula is A
1-xB
xEu
yAlSiN
3, x=0.0-0.5, y=0.001-0.2, B are Ca, Sr, one or more among the Ba.
Synthetic white light and backlight LED is characterized in that with the preparation method of nitride red fluorescent powder under a kind of normal pressure, and this method is according to following steps, with the A of 1.90-1.999 mole; 0.001-0.05 EuX3 (xF, Cl, Br, the I of mole; O) and 0.333 mole Si3N4, the solubility promoter NH4X (X=F, Cl) that adds the 0.01-0.10 mole; 1 mole AlN thorough mixing obtains mixture, in nitrogen among the 1300-2000 calcination 3-15 hour, is cooled to room temperature; Take out broken ball milling and washing, descended dry 5-12 hour at 120 degrees centigrade, product is through 200 eye mesh screens.Obtain white light LEDs and use nitride rouge and powder.Said compd A is CaN
2/3, SrN
2/3, BaN
zZ=0.01-6 or produce any other compound of this nitride
Synthetic white light and backlight LED are used nitride red fluorescent powder under a kind of normal pressure, it is characterized in that a kind of white light LEDs nitride rouge and powder, and emission wavelength ranges is the 580-680 nanometer.Excitation wavelength range is the 200-550 nanometer.
The chemistry and the thermostability of Nitride phosphor proposed by the invention are very good, and environmental protection.Assimilated efficiency is high, and very strong absorption is all arranged from the ultraviolet to the blue light, and the thermal quenching temperature is high.Its molecule is: the CaAlSiN3. emission peak is in the 580-680 nanometer, and excitation wavelength is from the 200-550 nanometer.
Advantage of the present invention:
1, the fluorescent material that composition through changing the matrix element and ratio can obtain the different emission peak value, making it becomes the red fluorescence powder from the orange-red fluorescent material of 580 nanometers to 680 nanometers, and its halfwidth also can change.
2, can change emissive porwer and chromaticity coordinates through regulating solubility promoter.
3, fluorescent material of the present invention can synthesize under normal pressure.
Fluorescent material of the present invention excites the very strong redness of emission down or orange red at blue light or ultraviolet LED chip.The backlight that can be widely used in white light LEDs and various display equipments cooperates other greens or yellow fluorescent powder can prepare the white light LEDs of high brightness high-color rendering or the LCD backlight source of high brightness high color purity.The invention provides the preparation method of this fluorescent material, its step and device requirement are simple.Synthesis under normal pressure, easy handling.
Fig. 1 is the emmission spectrum figure of sample
Fig. 2 is the exciting light spectrogram of sample
Fig. 3 is the x x ray diffration pattern x of sample
Specific embodiment
Embodiment one
Synthetic white light and backlight LED is characterized in that with the preparation method of nitride red fluorescent powder under a kind of normal pressure, and this method is according to following steps, with the CaN of 1.90-1.999 mole
2/3, 0.001 mole EuF
3Si with 0.333 mole
3N
4, 0.01 mole NH4Cl, 1 mole AlN thorough mixing obtains mixture, calcination 8 hours in 1600 degrees centigrade is cooled to room temperature in nitrogen, takes out broken ball milling and washing, 120 degrees centigrade dry 10 hours down, product is through 200 eye mesh screens.Obtain white light and backlight LED with nitride rouge and powder finished product.
Embodiment two
Synthetic white light and backlight LED is characterized in that with the method for feeling oneself inferior of nitride red fluorescent powder under a kind of normal pressure, and this method is according to following steps, with 1.998 moles CaN
2/3, the Si of 0.001 mole EuCl3 and 0.333 mole
3N
4, 0.01 mole NH4Cl, 1 mole AlN thorough mixing obtains mixture, calcination 8 hours in 1800 degrees centigrade is cooled to room temperature in nitrogen, takes out broken ball milling and washing, 120 degrees centigrade dry 10 hours down, product is through 200 eye mesh screens.Obtain white light and backlight LED with nitride rouge and powder finished product.
Embodiment three
Synthetic white light and backlight LED is characterized in that with the method for feeling oneself inferior of nitride red fluorescent powder under a kind of normal pressure, and this method is according to following steps, with 1.98 moles CaN
2/3, 0.01 mole SrN
2/3, the Si of 0.001 mole EuF3 and 0.333 mole
3N
4, 0.01 mole NH4Cl, 1 mole AlN thorough mixing obtains mixture, calcination 6 hours in 1800 degrees centigrade is cooled to room temperature in nitrogen, takes out broken ball milling and washing, 120 degrees centigrade dry 10 hours down, product is through 200 eye mesh screens.Obtain white light and backlight LED with nitride rouge and powder finished product.
Embodiment four
Synthetic white light and backlight LED is characterized in that with the method for feeling oneself inferior of nitride red fluorescent powder under a kind of normal pressure, and this method is according to following steps; Ca3N2 with 1.97 moles; 0.01 the SrN4 of mole, 0.01 mole BaNx, the Si of 0.001 mole EuCl3 and 0.333 mole
3N
4, 0.01 mole NH4Cl, 1 mole AlN thorough mixing obtains mixture, calcination 8 hours in 1650 degrees centigrade is cooled to room temperature in nitrogen, takes out broken ball milling and washing, 120 degrees centigrade dry 5 hours down, product is through 200 eye mesh screens.Obtain white light and backlight LED with nitride rouge and powder finished product.
Embodiment five
Synthetic white light and backlight LED is characterized in that with the method for feeling oneself inferior of nitride red fluorescent powder under a kind of normal pressure, and this method is according to following steps, with 1.90 moles CaN
2/3, the EuF3 of 0.001-0.05 mole (xF, Cl, Br, I is O) with 0.333 mole Si
3N
4, 0.01 mole NH4Cl, 1 mole AlN thorough mixing obtains mixture, calcination 8 hours in 1750 is cooled to room temperature in nitrogen, takes out broken ball milling and washing, 120 degrees centigrade dry 5 hours down, product is through 200 eye mesh screens.Obtain white light and backlight LED with nitride rouge and powder finished product.
Embodiment six
Synthetic white light and backlight LED is characterized in that with the method for feeling oneself inferior of nitride red fluorescent powder under a kind of normal pressure, and this method is according to following steps, with 1.98 moles CaN
2/3, the Si of 0.02 mole EuCl3 and 0.333 mole
3N
4, 0.01 mole NH4Cl, 1 mole AlN thorough mixing obtains mixture, calcination 8 hours in 1750 is cooled to room temperature in nitrogen, takes out broken ball milling and washing, 120 degrees centigrade dry 5 hours down, product is through 200 eye mesh screens.Obtain white light and backlight LED with nitride rouge and powder finished product.
Nitride red fluorescent powder chemical property of the present invention, the luminous efficiency height can be widely used in white light LEDs and backlight is used in demonstration.
Claims (5)
1. synthetic white light and backlight LED are used nitride red fluorescent powder under the normal pressure, and its molecular formula is A
1-xB
xEu
yAlSiN
3, x=0.0-0.5, y=0.001-0.2, A, B are Ca, Sr, one or more among the Ba.
2. synthetic white light and backlight LED is characterized in that with the preparation method of nitride red fluorescent powder this method is according to following steps, with the A of 1.90-1.999 mole under the normal pressure; 0.001-0.05 EuX3 (xF, Cl, Br, the I of mole; O) and 0.333 mole Si3N4, the solubility promoter NH4X (X=F, Cl) that adds the 0.01-0.1 mole; 1 mole AlN thorough mixing obtains mixture, in nitrogen among the 1300-2000 calcination 3-15 hour, is cooled to room temperature; Take out broken ball milling and washing, descended dry 5-12 hour at 120 degrees centigrade, product is through 200 eye mesh screens.Synthetic white light and backlight LED are used nitride rouge and powder under the acquisition normal pressure.Said compd A is CaN
2/3, SrN
2/3, BaN
zZ=0.01-6 maybe can produce any other compound of this nitride.
3. according to claim one, it is characterized in that synthetic white light and backlight LED nitride rouge and powder under a kind of normal pressure, emission wavelength ranges is the 580-680 nanometer, and excitation wavelength range is the 200-550 nanometer.
4. by the described a kind of fluorescent material of right 1 requirement, be encapsulated on the LED,, regulate colour temperature, optical parametrics such as chromaticity coordinates and brightness as white light LEDs.
5. by the described a kind of fluorescent material of right 1 requirement, be encapsulated on the LED, do the backlight of display device.
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| CN201010269713XA CN102382650A (en) | 2010-08-31 | 2010-08-31 | Nitride red phosphor synthesized at normal pressure for white light and backlight LED |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105181671A (en) * | 2015-09-21 | 2015-12-23 | 中国科学院长春光学精密机械与物理研究所 | Method for testing degree of ageing of nitride fluorescent powder |
| CN111170287A (en) * | 2020-02-07 | 2020-05-19 | 吉林大学 | High-temperature high-pressure preparation method of tetragonal strontium diazenium |
-
2010
- 2010-08-31 CN CN201010269713XA patent/CN102382650A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105181671A (en) * | 2015-09-21 | 2015-12-23 | 中国科学院长春光学精密机械与物理研究所 | Method for testing degree of ageing of nitride fluorescent powder |
| CN105181671B (en) * | 2015-09-21 | 2018-06-26 | 中国科学院长春光学精密机械与物理研究所 | The method for testing nitride phosphor degree of aging |
| CN111170287A (en) * | 2020-02-07 | 2020-05-19 | 吉林大学 | High-temperature high-pressure preparation method of tetragonal strontium diazenium |
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Application publication date: 20120321 |