CN103642492B - A kind of preparation method of silicon-based nitrogen oxide fluorescent powder - Google Patents
A kind of preparation method of silicon-based nitrogen oxide fluorescent powder Download PDFInfo
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- CN103642492B CN103642492B CN201310714968.6A CN201310714968A CN103642492B CN 103642492 B CN103642492 B CN 103642492B CN 201310714968 A CN201310714968 A CN 201310714968A CN 103642492 B CN103642492 B CN 103642492B
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 title claims abstract description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 13
- 239000010703 silicon Substances 0.000 title claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- YUJBNTKSQHVHAS-UHFFFAOYSA-N [Eu].C(C)C(=O)C(=O)C Chemical compound [Eu].C(C)C(=O)C(=O)C YUJBNTKSQHVHAS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 10
- TZMFJUDUGYTVRY-UHFFFAOYSA-N pentane-2,3-dione Chemical compound CCC(=O)C(C)=O TZMFJUDUGYTVRY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 239000002243 precursor Substances 0.000 claims abstract description 3
- 238000009413 insulation Methods 0.000 claims description 19
- 238000010792 warming Methods 0.000 claims description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- 239000012298 atmosphere Substances 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- AKTIAGQCYPCKFX-FDGPNNRMSA-L magnesium;(z)-4-oxopent-2-en-2-olate Chemical compound [Mg+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O AKTIAGQCYPCKFX-FDGPNNRMSA-L 0.000 claims description 6
- RUTFURLVCIRTKY-UHFFFAOYSA-N [Sr].C(C)C(=O)C(=O)C Chemical compound [Sr].C(C)C(=O)C(=O)C RUTFURLVCIRTKY-UHFFFAOYSA-N 0.000 claims description 2
- HYRVTHFPMWHAEG-SUKNRPLKSA-L barium(2+);(z)-4-oxopent-2-en-2-olate;hydrate Chemical compound O.[Ba+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O HYRVTHFPMWHAEG-SUKNRPLKSA-L 0.000 claims description 2
- QAZYYQMPRQKMAC-FDGPNNRMSA-L calcium;(z)-4-oxopent-2-en-2-olate Chemical compound [Ca+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O QAZYYQMPRQKMAC-FDGPNNRMSA-L 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims 3
- 239000000463 material Substances 0.000 abstract description 28
- 238000000034 method Methods 0.000 abstract description 15
- 150000004767 nitrides Chemical class 0.000 abstract description 14
- 239000000126 substance Substances 0.000 abstract description 11
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 8
- 230000002194 synthesizing effect Effects 0.000 abstract description 4
- 230000005284 excitation Effects 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 230000004913 activation Effects 0.000 abstract description 2
- 230000003712 anti-aging effect Effects 0.000 abstract description 2
- 238000006862 quantum yield reaction Methods 0.000 abstract description 2
- 239000007858 starting material Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 description 8
- 238000003786 synthesis reaction Methods 0.000 description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 5
- 238000009423 ventilation Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910002058 ternary alloy Inorganic materials 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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Abstract
A preparation method for silicon-based nitrogen oxide fluorescent powder, relates to a kind of preparation method of fluorescent material.By precursor raw material Polycarbosilane, methyl ethyl diketone europium, methyl ethyl diketone mixing, load after grinding in reaction vessel, after nitrogen replacement, under nitrogen atmosphere protection, after temperature reaction, naturally cool to room temperature; Products therefrom is ground, grinds again after sintering, obtain silicon-based nitrogen oxide fluorescent powder.Replace the pure metal, metal nitride etc. that use in current synthesizing nitride fluorescent material process expensive and the starting material of unstable chemcial property with the material of stable chemical nature, whole preparation process is simple; Required raw material variety is less, adopts different material rates, is equipped with the product that suitable process adjustments can obtain different performance; Simple to equipment requirements.Luminescent material is europkium-activated nitride, and quantum yield is high, and physical and chemical performance is stablized, and house anti-aging capability is excellent; Luminescent material excitation wavelength range is wide, can be suitable for the light source activation that multiple wave band excites.
Description
Technical field
The present invention relates to a kind of preparation method of fluorescent material, especially relate to a kind of preparation method of silicon-based nitrogen oxide fluorescent powder.
Background technology
Along with the progress of LED correlation technique, white light LEDs luminous efficiency, work-ing life, to reduce costs etc. in all make great progress.The shortcoming such as the low or color developing of the effective efficiency of conversion of current fluorescent material ubiquity used is poor, and the higher redness of efficiency of conversion and green emitting phosphor mostly are sulfide systems, its stability of photoluminescence is poor, light decay is larger.Therefore, the phosphor for white light LED developing efficient low light attenuation is extremely urgent.
Nitride phosphor is owing to having unique excitation spectrum (exciting scope to contain ultraviolet, near ultraviolet, blue light even green glow) and the characteristics of luminescence of excellence (launches green, yellow, ruddiness, hot-quenching go out little, luminous efficiency is high), it develops the very big concern receiving scientific circles and industrial community.Meanwhile, Nitride phosphor is nontoxic, good stability itself as the advantage of the novel luminescent material of a class, is applicable to very much being applied in the white light LEDs of white light LEDs particularly blue chip.Therefore, the measures and tactics of Development of Novel high-efficiency silicon nitride matter fluorescent powder has all successively been formulated in world many countries and area, to promote the development of its solid-state white LED, and makes every effort to obtain world-leading status in this regard.
Europkium-activated Nitride phosphor has high luminous efficiency and chemical stability is good, and excitation wavelength range is wide, and scope comprises all wave bands of blue light to ruddiness, is a kind of desirable LED fluorescent material.The method of conventional synthesizing nitride fluorescent material adopts the direct ammoniation process of metal; the method is raw materials used for synthesizing after the nitride metal of expensive, poor chemical stability; or adopt direct purchase price costly and the synthesis of the metal nitride of extremely unstable; this process must operate under the inert atmosphere protection in glove box; cost is high, complex process, is unfavorable for industrialized mass production.Current, batch production Nitride phosphor is mainly through simple substance element or the method preparation containing the multiple compounds mixed sintering of each element.To be raw material containing alkali-metal oxide compound, carbonate, nitrate, acetate, silicon-dioxide, compound, nitrate and carbon containing reducing substances containing europium disclosed in Chinese patent CN101798510A; low-temperature sintering in a nitrogen atmosphere after ball milling fully mixes, and then in protective atmosphere, improve the further high temperature sintering synthesis of sintering temperature.High temperature sintering temperature is up to 1800 degree, and the longest sintering time is 24h, and burning till product also needs to clean with the Virahol of upper volume through 3 times.Chinese patent CN102517000A is disclosed is raw material by alkali-metal simple substance or binary, ternary alloy or its halogenide, the silica flour that silicon source is got or beta-silicon nitride powder, it is raw material that rare earth metal gets simple substance, oxide compound or its alloy, under graphite furnace mesohigh nitrogen, high temperature sintering is carried out after abundant mixing, most high sintering temperature is 1800 degree, the highest nitrogen pressure is 1MPa, and sintering time is 12h.It is all harsher to raw material, equipment and synthesis condition that current conventional sintering prepares silicon-based nitrogen oxide fluorescent powder.And feed composition is too much, this makes the bad control of the performance of the finished product, is unfavorable for batch production.In addition, the quality of the simple substance such as High-purity Europium Metal, calcium, strontium or compound or purity also play conclusive impact to the performance of Nitride phosphor.
Summary of the invention
The object of the present invention is to provide that technique is simple, with short production cycle, reaction process is controlled, and the preparation method of a kind of silicon-based nitrogen oxide fluorescent powder that can be continuously produced.
The present invention includes following steps:
1) by precursor raw material Polycarbosilane, methyl ethyl diketone europium, methyl ethyl diketone mixing, load after grinding in reaction vessel, after nitrogen replacement, under nitrogen atmosphere protection, after temperature reaction, naturally cool to room temperature;
2) step 1) products therefrom is ground, grind again after sintering, obtain silicon-based nitrogen oxide fluorescent powder.
In step 1), the mass ratio of described Polycarbosilane, methyl ethyl diketone europium, methyl ethyl diketone can be (5 ~ 80): 1: (0 ~ 1); Described methyl ethyl diketone can be selected from the one in calcium acetylacetonate, methyl ethyl diketone strontium, acetylacetone barium, magnesium acetylacetonate etc.; The temperature of described temperature reaction can be 320 ~ 400 DEG C, and the time of temperature reaction can be 6 ~ 10h, and the speed of intensification can be 1 ~ 2 DEG C/min.
In step 2) in, the condition of described sintering puts into alumina crucible after can be and being ground by step 1) products therefrom, and in sintering oven, elder generation is to be warming up to 700 ~ 900 DEG C under ammonia atmosphere, and temperature rise rate is 1 ~ 2 DEG C/min, insulation 1 ~ 3h; Switch to nitrogen atmosphere, be warming up to 1350 ~ 1600 DEG C, temperature rise rate is 1 ~ 2 DEG C/min, insulation 1 ~ 3h.
Compared with prior art, the present invention has the following advantages:
(1) replace the pure metal, metal nitride etc. that use in current synthesizing nitride fluorescent material process expensive and the starting material of unstable chemcial property with the material of stable chemical nature, whole preparation process is simple;
(2) raw material variety needed for is less, adopts different material rates, is equipped with the product that suitable process adjustments can obtain different performance;
(3) simple to equipment requirements.Avoid hyperbaric environment required in building-up process, whole building-up process can be carried out in conventional containers and sintering oven, and process costs significantly reduces;
(4) luminescent material is europkium-activated nitride, and quantum yield is high, and physical and chemical performance is stablized, and house anti-aging capability is excellent;
(5) luminescent material excitation wavelength range is wide, can be suitable for the light source activation that multiple wave band excites.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the fluorescent material of preparation in the embodiment of the present invention 1.
Fig. 2 is the utilizing emitted light spectrogram of the fluorescent material of preparation in the embodiment of the present invention 1.
Fig. 3 is the utilizing emitted light spectrogram of the fluorescent material of preparation in the embodiment of the present invention 2.
Fig. 4 is the utilizing emitted light spectrogram of the fluorescent material of preparation in the embodiment of the present invention 3.
Fig. 5 is the utilizing emitted light spectrogram of the fluorescent material of preparation in the embodiment of the present invention 4.
Fig. 6 is the XRD figure of the fluorescent material of preparation in the embodiment of the present invention 5.
Fig. 7 is the utilizing emitted light spectrogram of the fluorescent material of preparation in the embodiment of the present invention 5.
Embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1:
With Polycarbosilane and methyl ethyl diketone europium for raw material, both mass ratioes are 5: 1.Two kinds of raw materials, after abundant mixed grinding 0.5h, put into three mouthfuls of vials, after fully substituting gas three times, under nitrogen atmosphere protection, are warming up to 320 DEG C with the speed of 1 DEG C/min, insulation 6h with nitrogen.Synthesis products therefrom, after abundant mixed grinding 0.5h, is put into alumina crucible, is filled ventilation three times, under ammonia atmosphere, be warming up to 800 DEG C with the speed of 1 DEG C/min, insulation 1h; Change nitrogen atmosphere, be warming up to 1350 DEG C with the speed of 1 DEG C/min, insulation 3h.Products therefrom after abundant grinding fluorescent material.Its XRD figure and utilizing emitted light spectrogram are see Fig. 1 and Fig. 2.
Embodiment 2:
With Polycarbosilane, methyl ethyl diketone europium and magnesium acetylacetonate for raw material, mass ratio is 20: 1: 0.2.Three kinds of raw materials carry out abundant mixed grinding 0.5h, put into three mouthfuls of vials, under nitrogen atmosphere protection, are warming up to 360 DEG C with the speed of 1 DEG C/min, insulation 6h.Synthesis products therefrom, after abundant mixed grinding 0.5h, is put into alumina crucible, is filled ventilation three times, under ammonia atmosphere, be warming up to 700 DEG C with the speed of 1 DEG C/min, insulation 3h; Change nitrogen atmosphere, be warming up to 1450 DEG C with the speed of 1 DEG C/min, insulation 3h.Products therefrom after abundant grinding fluorescent material.Its utilizing emitted light spectrogram is see Fig. 3.
Embodiment 3:
With Polycarbosilane, methyl ethyl diketone europium and magnesium acetylacetonate for raw material, mass ratio is 40: 1: 0.5.Three kinds of raw materials, after abundant mixed grinding 0.5h, put into three mouthfuls of vials, under nitrogen atmosphere protection, are warming up to 400 DEG C with the speed of 1 DEG C/min, insulation 6h.Synthesis products therefrom, after mixed grinding 0.5h, is put into alumina crucible, is filled ventilation three times, under ammonia atmosphere, be warming up to 900 DEG C with the speed of 1 DEG C/min, insulation 1h; Change nitrogen atmosphere, be warming up to 1550 DEG C with the speed of 1 DEG C/min, insulation 3h.Products therefrom after abundant grinding fluorescent material.Its utilizing emitted light spectrogram is see Fig. 4.
Embodiment 4:
With Polycarbosilane, methyl ethyl diketone europium and magnesium acetylacetonate for raw material, mass ratio is 80: 1: 1.Three kinds of raw materials, after abundant mixed grinding 0.5, put into three mouthfuls of vials, under nitrogen atmosphere protection, are warming up to 400 DEG C with the speed of 1 DEG C/min, insulation 6h.Synthesis products therefrom, after abundant mixed grinding 0.5h, is put into alumina crucible, is filled ventilation three times, under ammonia atmosphere, be warming up to 800 DEG C with the speed of 1 DEG C/min, insulation 1h; Change nitrogen atmosphere, be warming up to 1550 DEG C with the speed of 1 DEG C/min, insulation 3h.Products therefrom after abundant grinding fluorescent material.Its utilizing emitted light spectrogram is see Fig. 5.
Embodiment 5:
With Polycarbosilane, methyl ethyl diketone europium and magnesium acetylacetonate for raw material, mass ratio is 80: 1: 1.Three kinds of raw materials, after abundant mixed grinding 0.5, put into three mouthfuls of vials, under nitrogen atmosphere protection, are warming up to 360 DEG C with the speed of 1 DEG C/min, insulation 6h.Synthesis products therefrom, after abundant mixed grinding 0.5, is put into alumina crucible, is filled ventilation three times, under ammonia atmosphere, be warming up to 800 DEG C with the speed of 1 DEG C/min, insulation 1h; Change nitrogen atmosphere, be warming up to 1600 DEG C with the speed of 1 DEG C/min, insulation 3h.Products therefrom after abundant grinding fluorescent material.Its XRD figure and utilizing emitted light spectrogram are see Fig. 6 and 7.
Claims (3)
1. a preparation method for silicon-based nitrogen oxide fluorescent powder, is characterized in that comprising the following steps:
1) alkaline earth salt of precursor raw material Polycarbosilane, methyl ethyl diketone europium, methyl ethyl diketone is mixed, load in reaction vessel after grinding, after nitrogen replacement, under nitrogen atmosphere protection, after temperature reaction, naturally cool to room temperature; The mass ratio of the alkaline earth salt of described Polycarbosilane, methyl ethyl diketone europium, methyl ethyl diketone is 5 ~ 80: 1: 0 ~ 1;
2) by step 1) products therefrom grinding, grind again after sintering, obtain silicon-based nitrogen oxide fluorescent powder; The condition of described sintering is for by step 1) put into alumina crucible after products therefrom grinding, in sintering oven, first under ammonia atmosphere to be warming up to 700 ~ 900 DEG C, temperature rise rate is 1 ~ 2 DEG C/min, insulation 1 ~ 3h; Switch to nitrogen atmosphere, be warming up to 1350 ~ 1600 DEG C, temperature rise rate is 1 ~ 2 DEG C/min, insulation 1 ~ 3h.
2. the preparation method of a kind of silicon-based nitrogen oxide fluorescent powder as claimed in claim 1, is characterized in that in step 1) in, the alkaline earth salt of described methyl ethyl diketone is selected from the one in calcium acetylacetonate, methyl ethyl diketone strontium, acetylacetone barium, magnesium acetylacetonate.
3. the preparation method of a kind of silicon-based nitrogen oxide fluorescent powder as claimed in claim 1, is characterized in that in step 1) in, the temperature of described temperature reaction is 320 ~ 400 DEG C, and the time of temperature reaction is 6 ~ 10h, and the speed of intensification is 1 ~ 2 DEG C/min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2056366A1 (en) * | 2006-08-14 | 2009-05-06 | Fujikura, Ltd. | Light emitting device and illumination device |
| CN101724401A (en) * | 2008-10-21 | 2010-06-09 | 大连路明发光科技股份有限公司 | Red luminous silicon-oxygen nitride fluorescent material, preparation method and light emitting device using same |
| CN101962534A (en) * | 2010-08-11 | 2011-02-02 | 厦门大学 | Organic luminous material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2056366A1 (en) * | 2006-08-14 | 2009-05-06 | Fujikura, Ltd. | Light emitting device and illumination device |
| CN101724401A (en) * | 2008-10-21 | 2010-06-09 | 大连路明发光科技股份有限公司 | Red luminous silicon-oxygen nitride fluorescent material, preparation method and light emitting device using same |
| CN101962534A (en) * | 2010-08-11 | 2011-02-02 | 厦门大学 | Organic luminous material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| γ辐照聚碳硅烷先驱丝热解制备氮化硅陶瓷纤维及性能;黎阳等;《硅酸盐学报》;20131031;第41卷(第10期);第1318-1322页 * |
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