CN102382651A - Preparation method of nitride red fluorescent powder for light-emitting diodes - Google Patents
Preparation method of nitride red fluorescent powder for light-emitting diodes Download PDFInfo
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- CN102382651A CN102382651A CN2010102697252A CN201010269725A CN102382651A CN 102382651 A CN102382651 A CN 102382651A CN 2010102697252 A CN2010102697252 A CN 2010102697252A CN 201010269725 A CN201010269725 A CN 201010269725A CN 102382651 A CN102382651 A CN 102382651A
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Abstract
A preparation method of nitride red fluorescent powder for light-emitting diodes, which includes steps of reacting nitride of element A of an expression or any other compounds capable of generating the nitride, nitride or halide of the B or any other compounds capable of generating the nitride or the halide, nitride of Si or any other compounds capable of generating the nitride, nitride of Al or any other compounds capable of generating the nitride, and 0.1-5% of alkaline earth metal halide by molar concentration or NH4X (X referring to one or more of F, Cl and Br) at the temperature ranging from 1400 DEG C to 2000 DEG C in nitrogen or nitrogen and hydrogen mixed gas for three to ten hours, crushing and grinding after cooling to the ambient temperature, filtering by a 200-mesh screen, washing, and drying at 120 DEG C for five to ten hours.
Description
Technical field
The invention belongs to rare earth luminescent material and semiconductor light emitting field; Especially relate to a kind of fluorescent material with red-emitting of high brightness; A kind of method for preparing this red fluorescence powder, a kind of white light-emitting diodes, the backlight that a kind of various display equipments that use this red fluorescence powder are used.
Background technology
The luminous lighting source that is considered to 21 century a new generation of LED.It is a kind of semiconductor device that electric energy is converted into luminous energy.Have high light efficiency, energy-conservation, the life-span is long, and trigger voltage is low, antidetonation, advantages such as environmental protection.
Use blue-ray LED to apply the method that fluorescent material is the acquisition white light LEDs of at present widespread use.Its cost is low, makes simply, and luminous efficiency is high, is at present business-like effective technical.Generally speaking, all be to use to coat on emission blue light (wavelength is in the 450-470 nanometer) led chip can absorb this blue light and launch the fluorescent material of 540-570 nanometer, two kinds of light mix the back and form white lights.But because gold-tinted partly lacks red composition, cause present white light color developing relatively poor, can't satisfy the needs of general normal lighting.Therefore need to use and to remedy this defective at the blue-light excited fluorescent material that glows down of LED.
At present the rouge and powder that uses of white light LEDs is rare-earth activated sulfide, such as SrS:Eu. but this compounds is extremely unstable, decomposes easily, and the life-span is short.Cause chromaticity coordinates elegant and because the corrosion of S causes the inefficacy of led chip.At present the many of usefulness is nitride rouge and powder, its good stability, and brightness is high.Need high-temperature high-pressure apparatus but shortcoming is this compounds of preparation, and reaction raw materials is very responsive to humidity oxygen etc.
Summary of the invention
The present invention uses normal pressure equipment can prepare the red fluorescence powder that the LED of high brightness excites at high temperature, and the backlight that can be widely used in white light LEDs and all kinds of display equipments is used red fluorescence powder.
The LED that the present invention relates to uses the red fluorescence powder molecular formula to be: A2-xBxSi5-yAlyN8, and wherein A is earth alkali metal Ca, Sr; Among the Ba one or more, B are REE Eu, Sm; Ce, Tm, one or more .X=0.001-0.5 among the Dy; Y=0.001-4.999. its preparation method is, the nitride of the elements A in the expression maybe can be produced any other compound of this nitride, and nitride among the B or halogenide maybe can produce this nitride or halid any other compound; And the nitride of Si maybe can produce any other compound of this nitride, the nitride of Al or maybe can produce any other compound of this nitride, the alkaline earth metal halide of 0.1%-5% volumetric molar concentration or NH4X (x=F; Cl, Br) in one or more.
The red fluorescence powder, preparation method thereof that the present invention relates to is:
(1) nitride that takes by weighing an amount of corresponding A maybe can produce any other compound of such nitride; The category-B compound uses nitride or halogenide; Take by weighing Si, the Al nitride maybe can produce any other compound of such nitride, and adds the solubility promoter of 0.1%-5% volumetric molar concentration.X=0.001-0.5, y=0.001-4.999 changes.Uniform mixing.
(2) in the mixed gas of nitrogen or nitrogen hydrogen, reacted 3-10 hour at 1400-2000 degree centigrade.
(3) be cooled to room temperature, fragmentation is ground, cross 200 orders and shine net, washing, 120 degrees centigrade dry 5-10 hour down.Obtain the effective red fluorescence powder of a kind of light-emitting diodes
(4) at ultraviolet red-emitting under the exciting of blue-ray LED, peak wavelength is from the 590-680 nanometer, and with A, B composition and y value move.Luminous efficiency is high, and chemically stable is good.Can be used as white light LEDs and various display backlight LED encapsulation and use, change colour temperature and purity of color to improve color developing.
Advantage of the present invention
The present invention uses active height but stable initial reactant in the air, utilizes the little characteristics of halide anion radius in the reactant, has avoided the use high-tension apparatus.Only just can be that light emitting ionic gets in the lattice and luminous under the high temperature.
Figure of description
Fig. 1 is the emmission spectrum figure of embodiment one
Fig. 2 is the electron microscope picture of embodiment one
Embodiment one
A kind of LED uses red fluorescence powder, it is characterized by: take by weighing 1.98 moles SrN2/3,0.02 mole EuF3,1.67 moles Si3N4,0.01 mole NH4F.Uniform mixing.In nitrogen, reacted 10 hours at 1500 degrees centigrade.Be cooled to room temperature, fragmentation, grinding is crossed 200 orders and is shone net, washing, drying is 10 hours under 120 degrees centigrade.Obtain the effective red fluorescence powder of this kind light-emitting diodes.
Embodiment one
A kind of LED uses red fluorescence powder, it is characterized by: take by weighing 1.98 moles SrN2/3,0.02 mole EuF3,1.67 moles Si3N4,0.01 mole NH4F.Uniform mixing.In nitrogen, reacted 10 hours at 1500 degrees centigrade.Be cooled to room temperature, fragmentation, grinding is crossed 200 orders and is shone net, washing, drying is 10 hours under 120 degrees centigrade.Obtain the effective red fluorescence powder of this kind light-emitting diodes.
Embodiment two
A kind of LED uses red fluorescence powder, it is characterized by: take by weighing 1.98 moles SrN2/3,0.02 mole EuCl3,1.67 moles Si3N4,0.01 mole NH4Cl.Uniform mixing.In nitrogen, reacted 10 hours at 1500 degrees centigrade.Be cooled to room temperature, fragmentation, grinding is crossed 200 orders and is shone net, washing, drying is 10 hours under 120 degrees centigrade.Obtain the effective red fluorescence powder of this kind light-emitting diodes.
Embodiment three
A kind of LED uses red fluorescence powder, it is characterized by: take by weighing 1.88 moles SrN2/3,0.1 mole of CaN2/3,0.02 mole EuF3,1.67 moles Si3N4,0.02 mole NH4F.Uniform mixing.Reacted 10 hours at 1500 degrees centigrade at nitrogen.Be cooled to room temperature, fragmentation, grinding is crossed 200 orders and is shone net, washing, drying is 10 hours under 120 degrees centigrade.Obtain the effective red fluorescence powder of this kind light-emitting diodes.
Embodiment four
A kind of LED uses red fluorescence powder, it is characterized by: take by weighing 1.98 moles SrN2/3,0.02 mole EuCl3,1.67 moles Si3N4,0.01 mole AlN, 0.02 mole NH4Cl.Uniform mixing.In nitrogen, reacted 10 hours at 1500 degrees centigrade.Be cooled to room temperature, fragmentation, grinding is crossed 200 orders and is shone net, washing, drying is 10 hours under 120 degrees centigrade.Obtain the effective red fluorescence powder of this kind light-emitting diodes.
Embodiment five
A kind of LED uses red fluorescence powder, it is characterized by: the SrN that takes by weighing 1.98 moles
2/3, 0.02 mole EuF3,0.86 mole Si3N4,2.5 moles AlN, 0.01 mole NH4F.Uniform mixing.Reacted 10 hours at 1500 degrees centigrade at nitrogen.Be cooled to room temperature, fragmentation, grinding is crossed 200 orders and is shone net, washing, drying is 10 hours under 120 degrees centigrade.Obtain the effective red fluorescence powder of this kind light-emitting diodes.
Embodiment six
A kind of LED uses red fluorescence powder, it is characterized by: take by weighing 1.98 moles CaN2/3,0.02 mole EuF3,1.67 moles Si3N4,0.01 mole NH4F.Uniform mixing.In nitrogen, reacted 10 hours at 1500 degrees centigrade.Be cooled to room temperature, fragmentation, grinding is crossed 200 orders and is shone net, washing, drying is 10 hours under 120 degrees centigrade.Obtain the effective red fluorescence powder of this kind light-emitting diodes.
Claims (11)
1. a photodiode (LED) is used red fluorescence powder.It is characterized by this fluorescent material and have following molecular formula: A2-xBxSi5-yAlyN8.
2. by claim one, it is characterized by A is earth alkali metal Ca, Sr, and one or more among the Ba, raw material A is any other compound that nitride maybe can produce this nitride.
3. by claim one, it is characterized by B is REE Eu, and Sm, Ce, Tm, one or more among the Dy, raw material B are that nitride or halogenide maybe can produce this nitride or halid any other compound.
4. by claim one, it is characterized by X=0.001--0.5.
5. by claim one, it is characterized by y=0.001--4.999.
6. by claim one, it is characterized by, the reaction raw materials of elements Si is any other compound that the nitride of Si maybe can produce this nitride.
7. by claim one, it is characterized by, the reaction raw materials of elements Si is any other compound that the nitride of Al maybe can produce this nitride.
8. by claim one; It is characterized by, the preparation method is with raw material in the expression and the alkaline earth metal halide or NH4X (x=F, the Cl that add the 0.1%-5% volumetric molar concentration in addition; Br;) in one or more, uniform mixing, in the mixed gas of nitrogen or nitrogen hydrogen 1400-2000 degree centigrade the reaction 3-10 hour.
9. by claim one, this fluorescent material is at ultraviolet red-emitting under the exciting of blue-ray LED, and peak wavelength is from the 590-680 nanometer, with A, and B composition and x, the y value is mobile.
10. 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.
11. 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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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102697252A CN102382651A (en) | 2010-08-31 | 2010-08-31 | Preparation method of nitride red fluorescent powder for light-emitting diodes |
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| CN2010102697252A CN102382651A (en) | 2010-08-31 | 2010-08-31 | Preparation method of nitride red fluorescent powder for light-emitting diodes |
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| CN102382651A true CN102382651A (en) | 2012-03-21 |
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Application publication date: 20120321 |