CN102899038A - Nitride red fluorescent powder and preparation method thereof - Google Patents

Nitride red fluorescent powder and preparation method thereof Download PDF

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CN102899038A
CN102899038A CN2012104281880A CN201210428188A CN102899038A CN 102899038 A CN102899038 A CN 102899038A CN 2012104281880 A CN2012104281880 A CN 2012104281880A CN 201210428188 A CN201210428188 A CN 201210428188A CN 102899038 A CN102899038 A CN 102899038A
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fluorescent powder
red fluorescent
nitride red
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滕晓明
何锦华
梁超
符义兵
刘凯
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JIANGSU BORUI PHOTOELECTRIC CO Ltd
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Abstract

The invention discloses nitride red fluorescent powder. The chemical structural formula of the nitride red fluorescent powder is L2-x-y-zM5N8:Eux, Ry, R'z, wherein L is at least one of Ca, Sr or Ba; M is at least one of Si or Ge, and Si is requisite; R is at least one of Na or K; R' is at least one of La, Sm or Sc; and x is more than or equal to 0.001 and less than or equal to 0.5, y is more than or equal to 0.0001 and less than or equal to 0.01, z is more than or equal to 0.0001 and less than or equal to 0.01, and y is equal to z. The nitride red fluorescent powder is good in chemical stability, high in luminous efficiency and good in aging resistance; and the preparation method is simple, easy to operate, pollution-free and low in cost.

Description

A kind of nitride red fluorescent powder and preparation method thereof
Technical field
The present invention relates to a kind of nitride red fluorescent powder and preparation method thereof.
Background technology
Because potential application and the huge market of photodiode (LED), technology is maked rapid progress, so that luminous efficiency improves fast and the rapid decline of cost, the curtain in semiconductor lighting epoch is about to pull open.
Along with the arrival of the new LED lighting criteria of the U.S., the LED product quality is proposed requirements at the higher level, the parameters such as colour rendering index, correlated(color)temperature and life-span of particularly not too paying attention to now, this just has higher requirement to the performance of red fluorescence powder.
In existing red fluorescence powder, M 2Si 5N 8: Eu (M=Ca, Sr, Ba) more and more has been subject to investigator's attention owing to having good luminous efficiency and chemical stability.But because its structure itself, aging amplitude is larger in application process, can't practical requirement.
Technology contents
The invention provides a kind of nitride red fluorescent powder and preparation method thereof.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of nitride red fluorescent powder, its chemical structural formula is: L 2-x-y-zM 5N 8: Eu x, R y, R ' z, in the formula, L is at least a among Ca, Sr or the Ba; M is at least a among Si or the Ge, and wherein Si is necessary; R is at least a among Na or the K; R ' is at least a among La, Sm or the Sc; 0.001≤x≤0.5,0.0001≤y≤0.01,0.0001≤z≤0.01, and y=z.
The applicant studies discovery, and above-mentioned nitride can effectively be excited by ultraviolet, purple light or blue light.The applicant also finds, because Sr 2+With Eu 2+Ionic radius is close, and when adding basic metal and the metal ions such as La, Sm and Sc, the ion that differs greatly with the matrix ion radius under the high temperature is more easily separated out, and has guaranteed the inner Eu of product 2+Concentration is even; And the adding Alkali-Metal Na +And K +, both guaranteed also to have improved the charge balance of system product degree of crystallinity, thereby improved the aging resistance of product.
The preparation method of above-mentioned nitride red fluorescent powder may further comprise the steps:
A, press L 2-x-y-zM 5N 8: Eu x, R y, R ' zStoichiometric ratio take by weighing raw material, and mixing;
B, with the roasting of steps A gained material;
C, with step B gained crushing material, sieve, get nitride red fluorescent powder.
In order to enhance product performance, above-mentioned preparation method, also comprise step D, with the nitride red fluorescent powder of step C gained wash to specific conductivity less than the 10s/cm post-drying.
In order to improve detersive efficiency, above-mentioned washing is first pickling after washing, and used acid is a kind of in hydrochloric acid, nitric acid or the phosphoric acid during pickling, and the concentration of acid is 1-20wt%.
In order to enhance product performance, among the above-mentioned steps B, roasting is: under the normal pressure, in nitrogen atmosphere or the hydrogen nitrogen mixed gas atmosphere, divide two sections and carry out roasting: the maturing temperature of first paragraph is 700-900 ℃, roasting time is 4-8 hour, and the maturing temperature of second segment is 1400-1800 ℃, and the time of roasting is 8-15 hour.
In the above-mentioned hydrogen nitrogen mixed gas atmosphere, the volume ratio of hydrogen and nitrogen is (5:95)-(75:25).
In order to guarantee the performance of products obtained therefrom, in the steps A, the raw material of L, M, R ' element is their nitride, and the raw material of R element is its muriate, and the raw material of Eu element is its oxide compound.
Above-mentioned Nitride phosphor is encapsulated, be about to Nitride phosphor and YAG and mix by a certain percentage, and then by being coated in the blue chip surface after certain Ratio of filler bitumen mixing, namely can be made into white light LEDs.
Nitride phosphor chemical stability of the present invention is good, luminous efficiency is high, aging resistance good; And the preparation method is simple, and easy handling is pollution-free, cost is low.
Description of drawings
Fig. 1 is the exciting light spectrogram of embodiment 3 and comparative example 1.
Fig. 2 is the utilizing emitted light spectrogram of embodiment 3 and comparative example 1.
Fig. 3 is the XRD figure spectrum of embodiment 3 and comparative example 1.
Fig. 4 is the exciting light spectrogram of embodiment 7 and comparative example 2.
Fig. 5 is the utilizing emitted light spectrogram of embodiment 7 and comparative example 2.
Fig. 6 is the exciting light spectrogram of embodiment 10 and comparative example 3.
Fig. 7 is the utilizing emitted light spectrogram of embodiment 10 and comparative example 3.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1
Take by weighing Sr 3N 28.453g, Si 3N 410.735g, Eu 2O 30.808g, NaCl 0.0003g, LaN 0.0009g; above raw material is fully mixed, in the molybdenum crucible of packing into, move into rapidly it in tube furnace again; then under the protection of the mixed atmosphere (the hydrogen volume ratio is 10%) of nitrogen hydrogen, be warming up to gradually 800 ℃; be incubated 6 hours, and then be warming up to 1400 ℃, be incubated 10 hours; after grinding, sieving; nitric acid with 5% washs, and is 4.8 μ s/cm, oven dry with deionized water wash to specific conductivity at last, can make Sr 1.899Si 5N 8: Eu 0.1, Na 0.0005, La 0.0005Nitride phosphor.Its emission main peak and luminous intensity see Table 1, all are higher than comparative example 1.
Embodiment 2
Take by weighing Sr 3N 27.600g, Si 3N 410.735g, Eu 2O 30.808g, KCl 0.0086g, SmN 0.0189g; above raw material is fully mixed, in the molybdenum crucible of packing into, move into rapidly it in carbon tube furnace again; then under the protection of the mixed atmosphere (the hydrogen volume ratio is 10%) of nitrogen hydrogen, be warming up to gradually 800 ℃; be incubated 6 hours, and then be warming up to 1400 ℃, be incubated 10 hours; after grinding, sieving; hydrochloric acid with 12% washs, and is 5.6 μ s/cm, oven dry with deionized water wash to specific conductivity at last, can make Sr 1.88Si 5N 8: Eu 0.1, K 0.01, Sm 0.01Nitride phosphor.Its emission main peak and luminous intensity see Table 1, all are higher than comparative example 1.
Embodiment 3
Take by weighing Sr 3N 28.047g, Ca 3N 20.183g, Si 3N 410.781g, Eu 2O 30.811g, NaCl 0.0007g, ScN0.0007g; above raw material is fully being mixed, in the molybdenum crucible of packing into, moving into rapidly it in tube furnace again; then under the protection of pure nitrogen gas, be warming up to gradually 800 ℃; be incubated 6 hours, and then be warming up to 1400 ℃, be incubated 10 hours; after grinding, sieving; phosphoric acid with 8% washs, and is 7.3 μ s/cm, oven dry with deionized water wash to specific conductivity at last, can make Sr 1.818Ca 0.08Si 5N 8: Eu 0.1, Na 0.001, Sc 0.001Nitride phosphor.Its emission main peak and luminous intensity see Table 1, all are higher than comparative example 1.
Embodiment 4
Take by weighing Sr 3N 28.157g, Si 3N 410.633g, Eu 2O 30.799g, KCl 0.0086g, LaN 0.0087g; SmN0.0093g fully mixes above raw material, in the molybdenum crucible of packing into; again it is moved in the tube furnace rapidly, then under the protection of pure nitrogen gas, be warming up to gradually 800 ℃, be incubated 6 hours; and then be warming up to 1400 ℃; be incubated 10 hours, after grinding, sieving, the hydrochloric acid with 6% washs; be 5.2 μ s/cm, oven dry with deionized water wash to specific conductivity at last, can make Sr 1.88Si 5N 8: Eu 0.1, K 0.01, La 0.005, Sm 0.005Nitride phosphor.Its emission main peak and luminous intensity see Table 1, all are higher than comparative example 1.
Comparative example 1
Take by weighing Sr 3N 28.457g, Si 3N 410.735g, Eu 2O 30.808g; above raw material is fully mixed, in the molybdenum crucible of packing into, move into rapidly it in tube furnace again; then under the protection of the mixed atmosphere (the hydrogen volume ratio is 10%) of nitrogen hydrogen, be warming up to gradually 800 ℃; be incubated 6 hours, and then be warming up to 1400 ℃, be incubated 10 hours; after grinding, sieving; nitric acid with 5% washs, and is 6.1 μ s/cm, oven dry with deionized water wash to specific conductivity at last, can make Sr 1.9Si 5N 8: the Nitride phosphor of 0.1Eu, its emission main peak and luminous intensity see Table 1, and luminous intensity all is lower than each embodiment.
The prepared fluorescent material of all embodiment and comparative example and YAG press 0.14:1 and mix, and then mix being coated in the blue chip surface according to the Ratio of filler bitumen of 1:6, namely can be made into white light LEDs.Through its initial performance of test after the oven dry, then through its aging resistance of test behind 168 hours aging, see the following form 1:
Table 1
Figure BDA00002331473200041
Embodiment 5
Take by weighing Ca 3N 25.438g, Si 3N 410.735g, Eu 2O 30.0808g, NaCl 0.0007g, LaN 0.0017g; above raw material is fully mixed, in the molybdenum crucible of packing into, move into rapidly it in tube furnace again; then under the protection of the mixed atmosphere (the hydrogen volume ratio is 50%) of nitrogen hydrogen, be warming up to gradually 750 ℃; be incubated 4 hours, and then be warming up to 1450 ℃, be incubated 12 hours; after grinding, sieving; hydrochloric acid with 9% washs, and is 3.6 μ s/cm, oven dry with deionized water wash to specific conductivity at last, can make Ca 1.988Si 5N 8: Eu 0.01, Na 0.001, La 0.001Nitride phosphor.Its emission main peak and luminous intensity see Table 2, all are higher than comparative example 2.
Embodiment 6
Take by weighing Ca 3N 25.339g, Si 3N 410.735g, Eu 2O 30.0808g, KCl 0.0043g, SmN 0.0094g; above raw material is fully mixed, in the molybdenum crucible of packing into, move into rapidly it in tube furnace again; then under the protection of the mixed atmosphere (the hydrogen volume ratio is 50%) of nitrogen hydrogen, be warming up to gradually 750 ℃; be incubated 4 hours, and then be warming up to 1450 ℃, be incubated 12 hours; after grinding, sieving; nitric acid with 4% washs, and is 2.1 μ s/cm, oven dry with deionized water wash to specific conductivity at last, can make Ca 1.98Si 5N 8: Eu 0.01, K 0.005, Sm 0.005Nitride phosphor.Its emission main peak and luminous intensity see Table 2, all are higher than comparative example 2.
Embodiment 7
Take by weighing Ca 3N 25.285g, Si 3N 413.095g, Eu 2O 30.0811g, KCl 0.0034g, ScN 0.0027g; above raw material is fully mixed, in the molybdenum crucible of packing into, move into rapidly it in tube furnace again; then under the protection of pure nitrogen gas, be warming up to gradually 750 ℃; be incubated 4 hours, and then be warming up to 1450 ℃, be incubated 12 hours; after grinding, sieving; phosphoric acid with 8% washs, and is 5.7 μ s/cm, oven dry with deionized water wash to specific conductivity at last, can make Ca 1.982Si 5N 8: Eu 0.01, K 0.004, Sc 0.004Nitride phosphor.Its emission main peak and luminous intensity see Table 2, all are higher than comparative example 2.
Embodiment 8
Take by weighing Ca 3N 25.162g, Si 3N 413.201g, Eu 2O 30.0994g, NaCl 0.0001g, SmN 0.0002g; above raw material is fully mixed, in the molybdenum crucible of packing into, move into rapidly it in tube furnace again; then under the protection of pure nitrogen gas, be warming up to gradually 750 ℃; be incubated 4 hours, and then be warming up to 1450 ℃, be incubated 12 hours; after grinding, sieving; nitric acid with 12% washs, and is 5.3 μ s/cm, oven dry with deionized water wash to specific conductivity at last, can make Ca 1.9898Si 5N 8: Eu 0.01, Na 0.0001, Sm 0.0001Nitride phosphor.Its emission main peak and luminous intensity see Table 2, all are higher than comparative example 2.
Comparative example 2
Take by weighing Ca 3N 25.438g, Si 3N 413.543g, Eu 2O 30.1019g; above raw material is fully mixed in glove box, in the molybdenum crucible of packing into, move into rapidly it in tube furnace again; then under the protection of the mixed atmosphere (the hydrogen volume ratio is 50%) of nitrogen hydrogen, be warming up to gradually 750 ℃; be incubated 4 hours, and then be warming up to 1450 ℃, be incubated 12 hours; after grinding, sieving; hydrochloric acid with 9% washs, and is 3.3 μ s/cm, oven dry with deionized water wash to specific conductivity at last, and can make chemical constitution is Ca 1.99Si 5N 8: Eu 0.01Fluorescent material, its emission main peak and luminous intensity see Table 2, luminous intensity all is lower than each embodiment.
The prepared fluorescent material of all embodiment and comparative example and YAG press 0.2:1 and mix, and then mix being coated in the blue chip surface according to the Ratio of filler bitumen of 1:5, namely can be made into white light LEDs.Through its initial performance of test after the oven dry, then through its aging resistance of test behind 168 hours aging, see the following form 2:
Table 2
Figure BDA00002331473200051
Figure BDA00002331473200061
Embodiment 9
Take by weighing Ba 3N 28.7011g, Si 3N 48.972g, Eu 2O 32.702g, NaCl 0.0011g, LaN 0.0029g; above raw material is fully mixed, in the molybdenum crucible of packing into, move into rapidly it in tube furnace again; then under the protection of the mixed atmosphere (the hydrogen volume ratio is 25%) of nitrogen hydrogen, be warming up to gradually 900 ℃; be incubated 8 hours, and then be warming up to 1600 ℃, be incubated 15 hours; after grinding, sieving; phosphoric acid with 12% washs, and is 6.3 μ s/cm, oven dry with deionized water wash to specific conductivity at last, can make Ba 1.596Si 5N 8: Eu 0.4, Na 0.002, La 0.002Nitride phosphor.Its emission main peak and luminous intensity see Table 3, all are higher than comparative example 3.
Embodiment 10
Take by weighing Ba 3N 28.6131g, Si 3N 48.948g, Eu 2O 32.692g, NaCl 0.0028g, SmN 0.0079g; above raw material is fully mixed, in the molybdenum crucible of packing into, move into rapidly it in tube furnace again; then under the protection of the mixed atmosphere (the hydrogen volume ratio is 25%) of nitrogen hydrogen, be warming up to gradually 900 ℃; be incubated 8 hours, and then be warming up to 1600 ℃, be incubated 15 hours; after grinding, sieving; nitric acid with 9% washs, and is 4.8 μ s/cm, oven dry with deionized water wash to specific conductivity at last, can make Ba 1.59Si 5N 8: Eu 0.4Na 0.005Sm 0.005Nitride phosphor.Its emission main peak and luminous intensity see Table 3, all are higher than comparative example 3.
Embodiment 11
Take by weighing Ba 3N 28.2189g, Sr 3N 20.299g, Si 3N 49.014g, Eu 2O 32.712g, NaCl 0.0006g, ScN0.0006g; above raw material is fully mixed, in the molybdenum crucible of packing into, move into rapidly it in tube furnace again; then under the protection of pure nitrogen gas, be warming up to gradually 900 ℃; be incubated 8 hours, and then be warming up to 1600 ℃, be incubated 15 hours; after grinding, sieving; nitric acid with 8% washs, and is 6.2 μ s/cm, oven dry with deionized water wash to specific conductivity at last, can make Ba 1.518Sr 0.08Si 5N8:Eu 0.4, Na 0.001, Sc 0.001Nitride phosphor.Its emission main peak and luminous intensity see Table 3, all are higher than comparative example 3.
Embodiment 12
Take by weighing Ba 3N 28.6041g, Si 3N 48.943g, Eu 2O 32.692g, KCl 0.0057g, LaN 0.0087g; ScN0.0012g fully mixes above raw material, in the molybdenum crucible of packing into; again it is moved in the tube furnace rapidly, then under the protection of pure nitrogen gas, be warming up to gradually 900 ℃, be incubated 8 hours; and then be warming up to 1600 ℃; be incubated 15 hours, after grinding, sieving, the hydrochloric acid with 4% washs; be 8.1 μ s/cm, oven dry with deionized water wash to specific conductivity at last, can make Ba 1.584Si 5N 8: Eu 0.4, K 0.008, La 0.006Sc 0.002Nitride phosphor.Its emission main peak and luminous intensity see Table 3, all are higher than comparative example 3.
Comparative example 3
Take by weighing Ba 3N 28.7183g, Si 3N 48.972g, Eu 2O 32.702g; above raw material is fully mixed, in the molybdenum crucible of packing into, move into rapidly it in carbon tube furnace again; then under the protection of the mixed atmosphere (the hydrogen volume ratio is 25%) of nitrogen hydrogen, be warming up to gradually 900 ℃; be incubated 8 hours, and then be warming up to 1600 ℃, be incubated 15 hours; after grinding, sieving; phosphoric acid with 12% washs, and is 7.2 μ s/cm, oven dry with deionized water wash to specific conductivity at last, and can make chemical constitution is Ba 1.6Si 5N 8: Eu 0.4Fluorescent material, its emission main peak and luminous intensity see Table 3, luminous intensity all is lower than each embodiment.
The prepared fluorescent material of all embodiment and comparative example and YAG press 0.12:1 and mix, and then mix being coated in the blue chip surface according to the Ratio of filler bitumen of 1:8, namely can be made into white light LEDs.Through its initial performance of test after the oven dry, then through its aging resistance of test behind 168 hours aging, see the following form 3:
Table 3
Figure BDA00002331473200071

Claims (7)

1. nitride red fluorescent powder, it is characterized in that: its chemical structural formula is: L 2-x-y-zM 5N 8: xEu, yR, zR ', in the formula, L is at least a among Ca, Sr or the Ba; M is at least a among Si or the Ge, and wherein Si is necessary; R is at least a among Na or the K; R ' is at least a among La, Sm or the Sc; 0.001≤x≤0.5,0.0001≤y≤0.01,0.0001≤z≤0.01, and y=z.
2. the preparation method of nitride red fluorescent powder claimed in claim 1 is characterized in that: may further comprise the steps:
A, press L 2-x-y-zM 5N 8: Eu x, R y, R ' zStoichiometric ratio take by weighing raw material, and mixing;
B, with the roasting of steps A gained material;
C, with step B gained crushing material, sieve, get nitride red fluorescent powder.
3. the preparation method of nitride red fluorescent powder as claimed in claim 2 is characterized in that: also comprise step D, with the nitride red fluorescent powder of step C gained wash to specific conductivity less than 10 μ s/cm post-dryings.
4. the preparation method of nitride red fluorescent powder as claimed in claim 3, it is characterized in that: described washing is first pickling after washing, and used acid is hydrochloric acid, nitric acid or phosphoric acid during pickling, and the concentration of acid is 1-20wt%.
5. such as the preparation method of the described nitride red fluorescent powder of claim 2 to 4 any one, it is characterized in that: among the step B, roasting is: under the normal pressure, in nitrogen atmosphere or the hydrogen nitrogen mixed gas atmosphere, divide two sections and carry out roasting: the maturing temperature of first paragraph is 700-900 ℃, roasting time is 4-8 hour, and the maturing temperature of second segment is 1400-1800 ℃, and the time of roasting is 8-15 hour.
6. the preparation method of nitride red fluorescent powder as claimed in claim 5, it is characterized in that: in the described hydrogen nitrogen mixed gas atmosphere, the volume ratio of hydrogen and nitrogen is (5:95)-(75:25).
7. such as the preparation method of the described nitride red fluorescent powder of claim 2 to 4 any one, it is characterized in that: in the steps A, the raw material of L, M, R ' element is their nitride, and the raw material of R element is its muriate, and the raw material of Eu element is its oxide compound.
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CN109370587A (en) * 2018-09-06 2019-02-22 旭宇光电（深圳）股份有限公司 Nitride near-infrared fluorescent material, the light emitting device containing nitride near-infrared fluorescent material
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