CN103525409A - A high-luminous-efficiency high-stability nitride luminescent material and a manufacture method thereof - Google Patents

A high-luminous-efficiency high-stability nitride luminescent material and a manufacture method thereof Download PDF

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CN103525409A
CN103525409A CN201310465519.2A CN201310465519A CN103525409A CN 103525409 A CN103525409 A CN 103525409A CN 201310465519 A CN201310465519 A CN 201310465519A CN 103525409 A CN103525409 A CN 103525409A
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张书生
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Abstract

An objective of the invention is to provide a high-luminous-efficiency high-stability nitride luminescent material and a manufacture method thereof. The chemical formula of the nitride luminescent material is M[a-x]Al[b-y]A[y]D[c]N[3]:R[x], wherein the M element is one or more elements selected from Mg, Ca, Sr and Ba; the A element is one or two selected from V and P; the D element is one or more element selected from Si, Ge, Sn and Zr; the R element is one or more elements selected from Mn, Ce, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm and Yb; the a is not more than 1.5 and not less than 0.5; the x is not more than 0.5 and not less than 0.001; the b is not more than 1.5 and not less than 0.5; the y is not more than 0.5 and not less than 0.0001, the c is not more than 1.5 and not less than 0.5; and the nitride luminescent material has a crystal structure the same as CaAlSiN3. The nitride luminescent material has regular shapes, good consistency, the high luminous efficiency, the simple manufacturing method, and no pollution. The nitride luminescent material under excitation in a scope of ultraviolet, near ultraviolet, purple light and blue light has a broad-band luminescence spectrum the emitting main peak of which is ranging from 600 nm to 690 nm. A luminescent device prepared from the luminescent material has characteristics of a high luminous efficiency and a good color rendering property because the device is rich in high-luminous-efficiency red luminescent materials.

Description

A kind of high light efficiency, high stability nitride luminescent material and manufacture method thereof
Technical field:
The present invention relates to a kind of nitride luminescent material, be specifically related to a kind of a kind of improved nitride luminescent material that can effectively be excited by ultraviolet, near ultraviolet, purple light and blue light and preparation method thereof.
Background technology:
Photodiode (LED) has low voltage, high light efficiency, less energy-consumption, long lifetime, the advantage such as pollution-free, at semiconductor lighting and liquid crystal flat-panel demonstration field, is successfully applied.The implementation of white light LEDs is mainly divided into two kinds at present: the first is the combination of three primary colours (red, blue, green) LED chip; Another kind is to be mixed to form white light with LED fluorescence excitation thing, with blue-light LED chip, coordinate the fluorescent material of Yellow light-emitting low temperature, or two kinds of fluorescent material that coordinate glow green and red light with blue-ray LED, or with ultraviolet or three kinds of fluorescent material of purple LED de-excitation red, green, blue etc.In these implementations, blue-light LED chip coordinates simple, the easy row of the mode of YAG:Ce yellow fluorescent powder and relative low price, becomes the main flow scheme of white light LEDs.Yet make the white-light spectrum that forms in this way more single, spectrum mainly concentrates on gold-tinted region, cause the white light LEDs color developing of preparation lower.By add red fluorescence powder in encapsulation process, can compensate the red composition lacking in white light LEDs spectrum, improve the color developing of white light LEDs product.
But at present traditional red fluorescence powder is as sulfide and oxide compound etc., is not to exist the defects such as light decay is large, poor chemical stability, exactly because excite narrow range, cannot reach Perfect Matchings with LED chip.More traditional sulfide and the oxide compound of novel nitride red fluorescent powder had very large improvements in recent years, as CaAlSiN3:Eu and Ba2Si5N8:Eu have the wider emmission spectrum at 590-700nm, can mix being preferably equipped with blue chip and preparing high colour developing white light LEDs with YAG:Ce yellow fluorescent powder.But above-mentioned two kinds of Nitride phosphors all have shortcoming separately, as poor in the wet fastness of CaAlSiN3:Eu, its optical property under the condition of high humidity declines very fast, and the temperature tolerance of Ba2Si5N8:Eu is poor, and its optical property under the condition of high temperature declines very fast.Herein by the basis of CaAlSiN3:Eu, at Al 3+position on introduce V expandand P expandeffectively reduce Ca 2+position participates in Eu 2+impact on lattice, thereby chemical stability and the wet fastness of this structural material have greatly been improved, simultaneously, by adopting weakly reducing atmosphere and novel sintered mode in building-up process, thereby greatly reduce the impact of oxygen in building-up process, the light efficiency of this luminescent material is promoted, so this luminescent material have a good application prospect.
Summary of the invention:
The fluorescent material that the object of the present invention is to provide a kind of high light efficiency, high stability nitride luminescent material, can effectively be excited by ultraviolet, near ultraviolet, purple light and blue light.
Another object of the present invention is to provide a kind of under weakly reducing atmosphere the method for the simple above-mentioned fluorescent material of preparation.
The present invention takes following technical scheme: its chemical formula is: M a-xal b-ya yd cn 3: R xin formula, 0.5≤a≤1.5,0.001≤x≤0.5,0.5≤b≤1.5,0.0001≤y≤0.5,0.5≤c≤1.5, wherein M element is selected from one or more elements of Mg, Ca, Sr and Ba, and A element is selected from one or both of V and P, D element is selected from one or more elements of Si, Ge, Sn and Zr, and R element is selected from one or more elements of Mn, Ce, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm and Yb.
The preparation method of above-mentioned efficient, high stability nitride luminescent material, comprises the steps:
1) with the nitride of Mg, Ca, Sr, Ba, Al, Si, Ge, Sn, Zr, the nitride of Mn, Ce, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm and Yb or oxide compound, and the stoichiometric ratio forming by the chemical formula of structural formula (1) takes desired raw material;
2) above-mentioned raw materials is fully mixed in the atmosphere of nitrogen or argon gas;
3) said mixture is carried out in protective atmosphere to one or more snippets roasting;
4), again through aftertreatment, can be made into a kind of high brightness, high wet fastness nitride red fluorescent powder
5) be step 2) to mix in glove box.
6) step 3) protective atmosphere is the mixed atmosphere of hydrogen and nitrogen, and wherein hydrogen volume percentage composition is less than 10%.
7) step 3) pressure of protective atmosphere is 0.01Mpa-100Mpa.
8) one section of roasting step 3) is synthetic, and maturing temperature is 1470-1870 ℃, and roasting time is 5-22 hour.
9) the multistage roasting step 3) is synthetic, and first paragraph maturing temperature is 570-1170 ℃, and roasting time is 4-10 hour, and the maturing temperature of second segment is 1370-1770 ℃, and roasting time is 4-22 hour.
10) aftertreatment step 4) comprises grinding, pickling, washes, sieves, oven dry and classification.
11) acid that above-mentioned acid cleaning process adopts is nitric acid, and its mass concentration is 3%-15%.
12) according to claim 10) stage division described in described post-treating method is settling process, method of sieving, hydraulic classification or air classification.Tool of the present invention has the following advantages:
1. the innovative approach that a kind of nitride red luminescent material forms has been proposed, by the basis of CaAlSiN3:Eu, at Al 3+position on introduce V 3+and P 3+effectively reduce Ca 2+position participates in Eu 2+impact on lattice, thus chemical stability and the wet fastness of this structural material greatly improved.
2. proposed a kind of new synthetic schemes under weakly reducing atmosphere, thereby greatly reduced the impact of oxygen in building-up process, and then the light efficiency of this luminescent material is promoted, manufacture method is simple, and easy handling is pollution-free.
3. exciting light spectrum width, has transmitting main peak and is positioned at 600nm-690nm broad-band illumination spectrum under the exciting in ultraviolet, near ultraviolet, purple light and blue light range
4. can further make luminescent device, these white light emitting devices can be used widely in illumination or demonstration field.
Accompanying drawing explanation:
Fig. 1 is the excitation spectrum of embodiment 1;
Fig. 2 is the emmission spectrum of embodiment 1.
Embodiment
Be below embodiments of the invention, will contribute to further understanding of the invention, protection scope of the present invention is not limited to the examples, and its protection domain is decided by claim.
Comparative example 1
This comparative example's fluorescent material product, its chemical formula Sr 0.25ca 0.7alSiN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) also mixes, by the dusty raw materials mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein to mention percentage composition be 2% to nitrogen, gaseous tension is 0.1MPa, 1580 ℃ of insulations are after 15 hours, cool the temperature to below 80 ℃, after taking-up, grind, washing, sieve and dry the aftertreatments such as rear, the relative luminous intensity of gained fluorescent material and process humidity 85%, 85 ℃ of temperature, relative luminous intensity data after processing for 200 hours are as shown in table 1.
Embodiment 1
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.995v 0.005siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and V 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.
Embodiment 2
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.99v 0.01siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and V 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.
Embodiment 3
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.985v 0.015siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and V 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.
Embodiment 4
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.992p 0.008siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and P 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.
Embodiment 5
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.989p 0.011siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and P 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.
Embodiment 6
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.986p 0.014siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and P 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.
Embodiment 7
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.991v 0.003p 0.006siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and V 2o 3(analytical pure), P 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.Embodiment 8
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.988v 0.003p 0.009siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and V 2o 3(analytical pure), P 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.Embodiment 9
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.985v 0.003p 0.012siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and V 2o 3(analytical pure), P 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.Embodiment 10
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.988v 0.006p 0.006siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and V 2o 3(analytical pure), P 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.Embodiment 11
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.985v 0.006p 0.009siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and V 2o 3(analytical pure), P 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.Embodiment 12
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.982v 0.006p 0.012siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and V 2o 3(analytical pure), P 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.Embodiment 13
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.985v 0.009p 0.006siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and V 2o 3(analytical pure), P 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.Embodiment 14
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.982v 0.009p 0.009siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and V 2o 3(analytical pure), P 2o3 (analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.Embodiment 15
The present embodiment chemical formula is Sr 0.25ca 0.7al 0.979v 0.009p 0.012siN 3: Eu 0.05.Its manufacture method is for to take strontium nitride (4N) according to stoichiometric ratio, CaCl2 (4N), aluminium nitride (4N), silicon nitride (4N), nitrogenize europium (4N) and V 2o 3(analytical pure), P 2o 3(analytical pure), and mix, by the raw material mixing, under the mixed atmosphere of hydrogen and nitrogen, wherein hydrogen volume percentage composition is 3%, and gaseous tension is 0.01MPa, and 1530 ℃ of insulations are after 8 hours, cool the temperature to below 80 ℃, after taking-up, grind, wash, sieve and the aftertreatment such as oven dry, the relative luminous intensity of gained fluorescent material and through humidity 85%, 85 ℃ of temperature, the relative luminous intensity data after processing for 200 hours are as shown in table 1.
Table 1
Figure BSA0000095867770000041
Fluorescent material prepared by the present invention can be used for manufacturing white light LED luminescent device, detailed process is as follows: after fluorescent material of the present invention and other fluorescent material mixing are sized mixing, be coated on blue chip, weldering is turned on the electricity, by silica gel or resin package, gained solid state device is white light LED luminescent device.The kind of other fluorescent material that use and added amount thereof are determined according to product requirement.

Claims (8)

1. a nitride luminescent material, is characterized in that its chemical structural formula is as follows:
M a-xAl b-yA yD cN 3:R x (1)
In formula, 0.5≤a≤1.5,0.001≤x≤0.5,0.5≤b≤1.5,0.0001≤y≤0.5,0.5≤c≤1.5, wherein M element is selected from one or more elements of Mg, Ca, Sr and Ba, A element is selected from one or both of V and P, and D element is selected from one or more elements of Si, Ge, Sn and Zr, and R element is selected from one or more elements of Mn, Ce, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm and Yb.
2. the preparation method of nitride luminescent material described in claim 1, is characterized in that comprising the steps:
1) with the nitride of Mg, Ca, Sr, Ba, Al, Si, Ge, Sn, Zr, the nitride of Mn, Ce, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm and Yb or oxide compound, and the stoichiometric ratio forming by structural formula (1) chemical formula takes desired raw material;
2) said mixture raw material is mixed in the atmosphere of nitrogen or argon gas;
3) said mixture raw material is carried out in protective atmosphere to sintering;
4) intermediates after above-mentioned sintering are passed through to aftertreatment again, can be made into a kind of nitride red luminescent material.
3. preparation method according to claim 2, is characterized in that step 3) in, protective atmosphere is the mixed atmosphere of hydrogen and nitrogen, atmosphere pressures is 0.01MPa-100MPa.
4. preparation method according to claim 2, is characterized in that step 3) in, protective atmosphere is hydrogen nitrogen mixed gas atmosphere, wherein the volumn concentration of hydrogen is less than 10%.
5. preparation method according to claim 6, is characterized in that step 3) in, roasting adopts one or more snippets roasting.
6. preparation method claimed in claim 7, one section of roasting is synthetic, and maturing temperature is 1470-1870 ℃, and roasting time is 5-22 hour.
7. preparation method claimed in claim 7, multistage roasting is synthetic, and first paragraph maturing temperature is 570-1170 ℃, and roasting time is 4-10 hour, and the maturing temperature of second segment is 1370-1770 ℃, roasting time is 4-22 hour.
8. preparation method claimed in claim 2, is characterized in that 4) in, described aftertreatment comprises grinding, pickling, washes, sieves, oven dry and classification;
1) acid that acid cleaning process adopts is nitric acid, and its mass concentration is 3%-15%;
2) method that classification adopts is settling process, method of sieving, hydraulic classification or air classification.
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HIROMU WATANABE,ET AL.: "Synthetic Method and Luminescence Properties of SrxCa1−xAlSiN3:Eu2+ Mixed Nitride Phosphors", 《JOURNAL OF THE ELECTROCHEMICAL SOCIETY》 *
HIROMU WATANABE,ET AL.: "Synthetic Method and Luminescence Properties of SrxCa1−xAlSiN3:Eu2+ Mixed Nitride Phosphors", 《JOURNAL OF THE ELECTROCHEMICAL SOCIETY》, vol. 155, no. 3, 15 January 2008 (2008-01-15), pages 31 - 36, XP055157681, DOI: doi:10.1149/1.2829880 *

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* Cited by examiner, † Cited by third party
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CN104152144A (en) * 2014-03-28 2014-11-19 北京大学工学院包头研究院 Functional compound and preparation method thereof
CN104152144B (en) * 2014-03-28 2017-02-22 北京大学包头创新研究院 Functional compound and preparation method thereof
CN106634994A (en) * 2016-10-13 2017-05-10 河北利福光电技术有限公司 Nitride fluorescent powder and preparation method thereof
CN106929011A (en) * 2017-03-14 2017-07-07 河北利福光电技术有限公司 White emitting fluorescent powder that a kind of ultraviolet LED is excited and preparation method thereof
CN106929011B (en) * 2017-03-14 2019-04-23 河北利福光电技术有限公司 A kind of white emitting fluorescent powder and preparation method thereof of ultraviolet LED excitation
CN110157417A (en) * 2018-02-12 2019-08-23 有研稀土新材料股份有限公司 A kind of near infrared light luminescent material and the light emitting device comprising it
CN110157417B (en) * 2018-02-12 2022-05-10 有研稀土新材料股份有限公司 Near-infrared light luminescent material and luminescent device comprising same
CN110003903A (en) * 2019-04-11 2019-07-12 廊坊莱悦特电子科技有限公司 A kind of preparation method of inorganic nitride luminescent material
CN110003903B (en) * 2019-04-11 2021-09-03 廊坊莱悦特电子科技有限公司 Preparation method of inorganic nitride luminescent material
CN116376548A (en) * 2023-02-28 2023-07-04 江门市科恒实业股份有限公司 Silicon-aluminum-based red fluorescent powder and preparation method thereof
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