CN101914379A - Method for preparing nitrogen oxide phosphor powder - Google Patents
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- CN101914379A CN101914379A CN2010102412455A CN201010241245A CN101914379A CN 101914379 A CN101914379 A CN 101914379A CN 2010102412455 A CN2010102412455 A CN 2010102412455A CN 201010241245 A CN201010241245 A CN 201010241245A CN 101914379 A CN101914379 A CN 101914379A
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Abstract
The invention discloses a method for preparing nitrogen oxide phosphor powder. Salt and nitride of a metal component in the nitrogen oxide phosphor powder to be prepared are taken as raw materials, and the method comprises the following steps of: weighing the raw materials according to the stoichiometric proportion of the phosphor powder to be prepared, and dissolving the raw materials in water to prepare first suspension; adding a dispersant polyethylene glycol into the first suspension, fully dispersing the dispersant to prepare second suspension, and controlling the volume ratio of the dispersant to the first suspension to be 5-8:100; dropping ammonia water into the second suspension to make the pH value of the second suspension be 5-6; ultrasonically oscillating the second suspension in ultrasonic waves to prepare uniform and stable third suspension; putting the third suspension into a heating furnace, and performing thermal treatment at the temperature of between 500 and 600 DEG C for 2 to 3 hours to prepare precursor powder; and putting the precursor powder into a crucible, and calcining in the reducing atmosphere at the temperature of between 1,300 and 1,400 DEG C for 4.5 to 7 hours to prepare the required phosphor powder.
Description
Technical field
The present invention relates to the luminescent material technical field, be mainly used in the means of illumination such as cathode ray tube (CRT), field-emitter display (FED), plasma display (PDP), electroluminescent display unit such as (EL), fluorescent display tube, luminescent lamp, semiconductor lighting, relate in particular to the preparation method of the fluorescent powder of purple light～blue-light excited visible light or white light.
Background technology
White light LEDs is a kind of solid-state semiconductor device that converts electrical energy into white light, claim semiconductor lighting again, have the efficient height, plurality of advantages such as volume is little, the life-span is long, safety, low voltage, energy-saving and environmental protection, by people regard as after incandescent light, luminescent lamp, high-voltage gas discharging light the 4th generation lighting source, be the main product on the following illumination market.
Occurred various white light LEDs preparation methods at present, wherein blue-light LED chip and yellow fluorescent material combination, blue-light LED chip and redness and green fluorescent material combination, purple LED chip and fluorescent material with three basic colour make up the main method that these three kinds of methods are low with price, preparation simply becomes the preparation white light LEDs.The combination of blue-light LED chip and yellow fluorescent material is that to study also be the most sophisticated method the earliest, and the white light LEDs luminous efficiency of preparation is considerably beyond incandescent light, but colour rendering index is low, and the colour temperature height can not use as interior lighting.In order to improve the color developing of white light LEDs, the various countries scientist has researched and developed the methods that blue-light LED chip and red, green fluorescent material combination and purple LED chip and red, green, blue fluorescent material with three basic colour make up other two kinds of realization white light LEDs.Adopt the white light LEDs color developing of purple LED chip and fluorescent material with three basic colour combination to be improved significantly, but the high-level efficiency fluorescent material also relatively lacks, exist color to absorb again and proportioning regulation and control problem between the fluorescent material, and purple LED chip technology of preparing is immature, domesticly also be in the laboratory study stage, these factors cause near ultraviolet conversion hysteria white light LEDs to be difficult to obtain large-scale application in a short time.The mode that blue-light LED chip excites is red, the green fluorescence material obtains white light LEDs has the advantage of preceding dual mode: employing be blue-light LED chip, this type of chip is studied maturation both at home and abroad, has obtained large-scale application; The blue light that is sent by chip mixes with ruddiness and the green glow that fluorescent material is changed out, generates white light, has good color reducibility, meets the human vision requirement.
Will seek out fast development by white light LEDs red, the preparation of green fluorescent material coupling blue-light LED chip, one of them key factor is to obtain high quality red, green fluorescent material.Can sulfide, nitride, molybdate and silicate etc. be arranged by blue-light excited red, green fluorescent material at present.Sulfide luminescent material is the main raw in red, the green fluorescence material, as (Ca
1-xSr
x) S:Eu
2+Red fluorescence material, Ga
2S
3: Eu
2+Green fluorescent material, but sulfide instability at high temperature decompose easily, the toxigenicity material, and the white light LEDs life-span of preparation is short, and does not meet environmental requirement.People have developed Sr again
2Si
5N
8: Eu
2+Deng nitride fluorescent material, these materials have good fluorescent characteristic, but easy and air and steam reaction of alkaline-earth nitride in the raw material, complicated process of preparation, the powder purity that makes is low, at present can't scale operation.The luminescent material that with silicate is matrix has good chemical stability and thermostability, and the high-purity silicon dioxide raw material inexpensive, be easy to get, maturing temperature more and more is subjected to people and payes attention to than characteristics such as aluminates system are low, Sr occurred
2SiO
4: Eu
2+, CaMgSi
2O
7: Eu
2+Deng fluorescent material, wherein blue-light excited yellow fluorescent material Sr
3SiO
5: Eu
2+Luminous efficiency can compare favourably with YAG, and Lumi-tech company limited has been used to encapsulate white light LEDs, but the blue-light excited present efficient of red, green silicate fluorescent material is also lower, needs further improvement.
Nitric oxide fluorescent powder is because its unique excitation spectrum (exciting scope to contain ultraviolet, near ultraviolet, blue light even green glow) and the excellent characteristics of luminescence (are launched green, yellow, ruddiness; That hot-quenching is gone out is little, luminous efficiency is high), therefore nontoxic, the good stability of material itself is very suitable for being applied in the white light LEDs, the particularly application of the white light LEDs of blue chip, thereby received the very big concern of scientific circles and industrial community.
Because the oxynitride system contains nitrogen, so the synthetic of it need to adopt nitrogenous raw material or introduce nitrogen by nitrogen atmosphere, causes its synthetic being very limited.The preparation method about nitrogen oxide phosphor powder of report mainly is a solid reaction process in the world at present, and this method adopts Si usually
3N
4With AlN be initial feed because it has very strong covalent linkage, spread coefficient is low, reactive behavior is poor, therefore need be than higher calcining temperature (1600-2000 ℃) even reaction pressure (5-10atm).These composite factors cause the preparation process complexity of nitrogen oxide phosphor powder, manufacturing cost height.And the preparation of the luminescent powder of the feasible preparation of high synthesis temperature often produces hard aggregation, and particle thick (＞10 μ m) also needs to carry out aftertreatments such as ball mill pulverizing usually, and this certainly will introduce textural defect, reduces its luminous efficiency and stability.
Relevant solid reaction process can be Chinese patent and the following document of ZL 200510025004.6 referring to the patent No.:
(1)Volker?Bachmann，Andries?Meijerink，Cees?Ronda，Journal?ofLuminescence?129(2009)1341-1346；
(2)Rong-Jun?Xie，Naoto?Hirosaki，Ken?Sakuma，Yoshinobu?Yamamotoand?Mamoru?Mitomo，APPLIED?PHYSICS?LETTERS，Vol.84，No.26，28?June?2004；
(3)K.Sakuma，N.Hirosaki，R.-J.Xie，Y.Yamamoto，T.Suehiro，Materials?Letters?61(2007)547-550。
The vapour phase reduction nitriding is a kind of novel method for preparing meticulous two component system nitride powder that latest developments are got up, this method is from oxide raw material cheap and easy to get, adopt wet chemical technology at first to prepare the nano-oxide precursor, then by the synthetic meticulous two component system nitride of vapour phase reduction nitride-oxide precursor.With the advantage of this method is exactly that the granular size of precursor remains behind gas-solid phase reaction, so the size and the pattern of granular precursor controlled well just can be cut out (referring to T.Suehiro the granularity and the pattern of product, J.Tatami, T.Meguro, S.Matsuo, K.Komeya, J.Eur.Ceram.Soc.22 (2002) 521).At present, prepare polynary system nitrogen oxide phosphor powder (ask for an interview application number be 200910056464.3 Chinese patent application) about adopting this method, the nitriding atmosphere of employing mainly is ammonia and hydrocarbon gas gas mixture, has increased the preparation difficulty.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method for preparing nitrogen oxide phosphor powder.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: this method for preparing nitrogen oxide phosphor powder is to comprise the steps:
(1) salt and the nitride in the described nitric oxide fluorescent powder with the metal ingredient in the nitric oxide fluorescent powder that will prepare is raw material, according to described each raw material of the stoichiometric ratio weighing of the nitric oxide fluorescent powder that will prepare, then with water-soluble first suspension of making of each raw material;
(2) add dispersion agent in first suspension, described dispersion agent is well dispersed in obtains second suspension in first suspension, the volume ratio of the described dispersion agent and first suspension is 5～8: 100, and described dispersion agent is a polyoxyethylene glycol; Splash into ammoniacal liquor in second suspension, the pH value that makes described second suspension is 5～6;
(3) in ultrasonic wave, second suspension is carried out sonic oscillation, obtain homogeneous, stable the 3rd suspension;
(4) the 3rd suspension is put into process furnace, under 500～600 ℃ of temperature condition, carry out 2～3 hours thermal treatment, obtain precursor powder;
(5) described precursor powder is contained in the crucible, under 1300～1400 ℃ temperature, in reducing atmosphere, calcines and obtained needed fluorescent powder in 4.5～7 hours.
Further, the nitride in the nitric oxide fluorescent powder of the present invention is silicon nitride and/or aluminium nitride.
Further, the salt of metal ingredient is the nitrate or the hydrochloride of this metal ingredient in the nitric oxide fluorescent powder of the present invention.
Further, reducing atmosphere of the present invention is that 5% hydrogen and volumn concentration are that 95% nitrogen is formed by volumn concentration.
Compared with prior art, the invention has the beneficial effects as follows: (1) is at the shortcoming of solid reaction process and the existence of gas-phase reaction nitriding, the present invention adopts the fluorescent powder good uniformity of wet chemistry method preparation, especially the polycomponent fluorescent powder of the inventive method preparation, its uniformity coefficient can reach molecule or atomic level, active ions are evenly distributed in the lattice, can improve effective doping content, help strengthening the luminous intensity of sample.(2) calcining temperature of the present invention is lower than the solid phase method reaction of prior art, but save energy also can be avoided introducing impurity because calcining temperature is high from reactor; The product purity height.(3) the vapour phase reduction nitriding prepared nitrogen oxide phosphor powder of prior art needs to come nitrogenize precursor oxide compound with the gas mixture of the ammonia and the hydrocarbon gas as nitriding atmosphere, because the nitridation process severe reaction conditions has increased the preparation difficulty; And therefore the present invention need not the nitrogenize starting raw material owing to contain nitrogen, oxygen composition in raw material in preparation process, has simplified preparation technology.(4) the present invention is by adding dispersion agent, solved the problem of the water insoluble and organic solvent of nitride.(5) in addition, the present invention adopts ultrasonic technology, the purity and the granular size of the uniform mixing and the fluorescent powder of raw material have been guaranteed, prepared fluorescent powder need not ground substantially, reduce postprocessing working procedures the destruction of the crystalline network of fluorescent powder is reduced luminous efficiency, and the products obtained therefrom pattern is better.
Description of drawings
Fig. 1 is X-ray powder diffraction (XRD) figure of the fluorescent powder of the embodiment of the invention 1 preparation;
Fig. 2 is scanning electron microscope (SEM) figure of the fluorescent powder of the embodiment of the invention 1 preparation;
Fig. 3 is the exciting and emmission spectrum of fluorescent powder of the embodiment of the invention 1 preparation;
Fig. 4 is X-ray powder diffraction (XRD) figure of the fluorescent powder of the embodiment of the invention 2 preparations.
Embodiment
Embodiment 1:
In the present embodiment, the nitric oxide fluorescent powder that prepare is (Y
5.9Ce
0.1) Si
3O
9N
4, wherein, metal ingredient is Y and Ce, nitride is Si
3N
4According to (Y
5.9Ce
0.1) Si
3O
9N
4Take by weighing the nitrate Y (NO of Y
3)
36H
2O (AR) 22.5976 grams, the nitrate Ce (NO of Ce
3)
36H
2O (99.99%) 0.4342 gram and nitride Si
3N
4(AR) 1.4028 grams are dissolved in the distilled water, and thorough mixing is made 100ml milk-white coloured suspension A; In suspending liquid A, add the 5ml polyoxyethylene glycol, fully stir, obtain suspension B; Splash into ammoniacal liquor, regulate the pH of suspension B, keeping pH is 6.In ultrasonic wave, suspension B is carried out sonic oscillation 30 minutes, obtain homogeneous, steady suspension C; C puts into retort furnace with suspension, carries out 2 hours thermal treatment under 500 ℃ of temperature condition, obtains precursor powder D; Precursor powder D is contained in the plumbago crucible, and in reducing atmosphere calcining 7 hours, the hydrogen that consists of 5% volumn concentration of reducing atmosphere and the nitrogen of 95% volumn concentration promptly obtained needed fluorescent powder (Y under 1300 ℃ of temperature
5.9Ce
0.1) Si
3O
9N
4X-ray diffraction shows d value and the relative intensity variation tendency and the Y of products therefrom
6Si
3O
9N
4The consistent (see figure 1) of standard card (JCPDSNo 30-1461); The position of excitation peak is at 385nm and 420nm, and the position of emission peak is in the 536nm (see figure 3).And as shown in Figure 2, the particle of fluorescent material is less, is about 5 μ m, and the particles dispersed of fluorescent material is good, need not the later stage attrition process.
Embodiment 2:
In the present embodiment, the nitric oxide fluorescent powder that prepare is (Y
5.5Ce
0.5) Si
3O
9N
4, wherein, metal ingredient is Y and Ce, nitride is Si
3N
4, according to (Y
5.5Ce
0.5) Si
3O
9N
4Take by weighing the hydrochloride YCl of Y
36H
2O (AR) 25.0272 grams, the hydrochloride CeCl of Ce
36H
2O (99.99%) 2.6590 gram and nitride Si
3N
4(AR) 2.1042 grams are dissolved in the distilled water, and thorough mixing is made 100ml milk-white coloured suspension A; In suspending liquid A, add the 5ml polyoxyethylene glycol, fully stir, obtain suspension B, splash into ammoniacal liquor again, regulate the pH of suspension B, and the pH that remains suspension B is 6.In ultrasonic wave, suspension B is carried out sonic oscillation 30 minutes, obtain homogeneous, steady suspension C; C puts into retort furnace with suspension, carries out 2.5 hours thermal treatment under 500 ℃ of temperature condition, obtains precursor powder D; Precursor powder D is contained in the plumbago crucible, and the reducing atmosphere calcining is 7 hours under 1300 ℃ of temperature, and reducing atmosphere is the hydrogen of 5% volumn concentration and the nitrogen of 95% volumn concentration, promptly obtains needed fluorescent powder (Y
5.5Ce
0.5) Si
3O
9N
4X-ray diffraction shows d value and the relative intensity variation tendency and the Y of this product
6Si
3O
9N
4The consistent (see figure 4) of standard card (JCPDS No30-1461).And the particle of fluorescent material is less, good dispersity, need not the later stage attrition process.
Embodiment 3:
In the present embodiment, the nitric oxide fluorescent powder that prepare is (Sr
0.9Yb
0.1) SiAl
2N
2O
3, wherein, metal ingredient is Sr, Al and Yb, nitride is Si
3N
4And AlN, according to (Sr
0.9Yb
0.1) SiAl
2N
2O
3Take by weighing the nitrate Sr (NO of Sr
3)
2(AR) 5.7140 grams, the nitrate Al (NO of Al
3)
36H
2O (AR) 15.0056 grams, the nitrate Yb (NO of Yb
3)
35H
2O (99.99%) 1.3474 gram, nitride Si
3N
4(AR) 1.4028 grams, nitride AlN (AR) 0.8198 gram is dissolved in the distilled water, and thorough mixing is made 100ml milk-white coloured suspension A; In suspending liquid A, add the 8ml polyoxyethylene glycol, fully stir, obtain suspension B, splash into ammoniacal liquor, the pH value of regulator solution, and the pH value of maintenance suspension B is 6.In ultrasonic wave, suspension B is carried out sonic oscillation 30 minutes, obtain homogeneous, steady suspension C; C puts into retort furnace with suspension, carries out 3 hours thermal treatment under 500 ℃ of temperature condition, obtains precursor powder D; Precursor powder D is contained in the plumbago crucible, and the reducing atmosphere calcining is 4.5 hours under 1400 ℃ of temperature, and reducing atmosphere is the hydrogen of 5% volumn concentration and the nitrogen of 95% volumn concentration, promptly obtains needed fluorescent powder (Sr
0.9Yb
0.1) SiAl
2N
2O
3The d value of gained fluorescent material and relative intensity variation tendency and SrSiAl
2N
2O
3Standard card (JCPDS No 88-1522) unanimity, and fluorescent powder grain is less, good dispersity, need not the later stage attrition process.
Embodiment 4:
In the present embodiment, the nitric oxide fluorescent powder that prepare is (Sr
0.7Yb
0.3) SiAl
2N
2O
3, wherein, metal ingredient is Sr, Al and Yb, nitride is Si
3N
4And AlN, according to (Sr
0.9Yb
0.1) SiAl
2N
2O
3Take by weighing the hydrochloride SrCl of Sr
2(AR) 6.6610 grams, the hydrochloride AlCl of Al
3(AR) 10.6680 grams, the hydrochloride YbCl of Yb
3(99.99%) 5.0290 gram, nitride Si
3N
4(AR) 2.8058 grams, nitride AlN (AR) 1.6396 grams are dissolved in the distilled water, and thorough mixing is made 100ml milk-white coloured suspension A; Add the 6ml polyoxyethylene glycol in suspending liquid A, fully stir, obtain suspension B, splash into ammoniacal liquor, regulate the pH of suspension B, keeping the pH of suspension B is 6.In ultrasonic wave, suspension B is carried out sonic oscillation 30 minutes, obtain homogeneous, steady suspension C.C puts into retort furnace with suspension, carries out 2 hours thermal treatment under 600 ℃ of temperature condition, obtains precursor powder D; Precursor powder D is contained in the plumbago crucible, and the reducing atmosphere calcining is 4.5 hours under 1400 ℃ of temperature, and reducing atmosphere is the hydrogen of 5% volumn concentration and the nitrogen of 95% volumn concentration, promptly obtains needed fluorescent powder (Sr
0.7Yb
0.3) SiAl
2N
2O
3The d value of gained fluorescent material and relative intensity variation tendency and SrSiAl
2N
2O
3Standard card (JCPDS No 88-1522) unanimity, and fluorescent powder grain is less, good dispersity, need not the later stage attrition process.
Embodiment 5
In the present embodiment, the nitric oxide fluorescent powder that prepare is (Ca
1.8Eu
0.2) Si
3O
2N
4, wherein, metal ingredient is Ca and Eu, nitride is Si
3N
4, according to (Ca
1.8Eu
0.2) Si
3O
2N
4Take by weighing the nitrate Ca (NO of Ca
3)
24H
2O (AR) 7.0028 grams, the nitrate Eu (NO of Eu
3)
36H
2O (99.99%) 3.5686 gram, nitride Si
3N
4(AR) 5.6112 grams are dissolved in the distilled water, and thorough mixing is made 100ml milk-white coloured suspension A; Add the 5ml polyoxyethylene glycol in suspending liquid A, fully stir, obtain suspension B, splash into ammoniacal liquor, regulate the pH of suspension B, keeping the pH of suspension B is 6.In ultrasonic wave, suspension B is carried out sonic oscillation 45 minutes, obtain homogeneous, steady suspension C.C puts into retort furnace with suspension, carries out 3 hours thermal treatment under 600 ℃ temperature condition, obtains precursor powder D.Precursor powder D is contained in the plumbago crucible, and the reducing atmosphere calcining is 7 hours under 1400 ℃ of temperature, and reducing atmosphere is the hydrogen of 5% volumn concentration and the nitrogen of 95% volumn concentration, promptly obtains needed fluorescent powder (Ca
1.8Eu
0.2) Si
3O
2N
4The d value of gained fluorescent material and relative intensity variation tendency and Ca
2Si
3O
2N
4Standard card (JCPDS No38-0945) unanimity, and fluorescent powder grain is less, good dispersity, need not the later stage attrition process.
Embodiment 6
In the present embodiment, the nitric oxide fluorescent powder that prepare is (Ba
0.9Eu
0.1) Al
11O
16N, wherein, metal ingredient is Ba, Al and Eu, nitride is AlN, according to (Ba
0.9Eu
0.1) Al
11O
16N takes by weighing the hydrochloride BaCl of Ba
2(AR) 0.9371 gram, the nitrate Al (NO of Al
3)
36H
2O (AR) 18.7570 grams, the nitrate Eu (NO of Eu
3)
36H
2O (99.99%) 0.2230 gram, nitride AlN (AR) 0.2050 gram is dissolved in the distilled water, and thorough mixing is made 100ml milk-white coloured suspension A; Add the 7ml polyoxyethylene glycol in suspending liquid A, fully stir, obtain suspension B, splash into ammoniacal liquor, regulate the pH of suspension B, keeping the pH of suspension B is 5.In ultrasonic wave, suspension B is carried out sonic oscillation 30 minutes, obtain homogeneous, steady suspension C.C puts into retort furnace with suspension, carries out 2.5 hours thermal treatment under 550 ℃ temperature condition, obtains precursor powder D.Precursor powder D is contained in the plumbago crucible, and the reducing atmosphere calcining is 4.5 hours under 1300 ℃ of temperature, and reducing atmosphere is the hydrogen of 5% volumn concentration and the nitrogen of 95% volumn concentration, promptly obtains needed fluorescent powder (Ba
0.9Eu
0.1) Al
11O
16N.The d value of gained fluorescent material and relative intensity variation tendency and BaAl
11O
16N standard card (JCPDS No 48-1821) unanimity, and fluorescent powder grain is less, good dispersity, need not the later stage attrition process.
The foregoing description is used for the present invention that explains, rather than limits the invention, and in the protection domain of spirit of the present invention and claim, any modification and change to the present invention makes all fall into protection scope of the present invention.
Claims (4)
1. a method for preparing nitrogen oxide phosphor powder is characterized in that comprising the steps:
(1) salt and the nitride in the described nitric oxide fluorescent powder with the metal ingredient in the nitric oxide fluorescent powder that will prepare is raw material, according to described each raw material of the stoichiometric ratio weighing of the nitric oxide fluorescent powder that will prepare, then with water-soluble first suspension of making of each raw material;
(2) add dispersion agent in first suspension, described dispersion agent is well dispersed in obtains second suspension in first suspension, the volume ratio of the described dispersion agent and first suspension is 5～8: 100, and described dispersion agent is a polyoxyethylene glycol; Splash into ammoniacal liquor in second suspension, the pH value that makes described second suspension is 5～6;
(3) in ultrasonic wave, second suspension is carried out sonic oscillation, obtain homogeneous, stable the 3rd suspension;
(4) the 3rd suspension is put into process furnace, under 500～600 ℃ of temperature condition, carry out 2～3 hours thermal treatment, obtain precursor powder;
(5) described precursor powder is contained in the crucible, under 1300～1400 ℃ temperature, in reducing atmosphere, calcines and obtained needed fluorescent powder in 4.5～7 hours.
2. the method for preparing nitrogen oxide phosphor powder according to claim 1 is characterized in that: the nitride in the described nitric oxide fluorescent powder is silicon nitride and/or aluminium nitride.
3. the method for preparing nitrogen oxide phosphor powder according to claim 1 and 2 is characterized in that: the salt of metal ingredient is the nitrate or the hydrochloride of this metal ingredient in the described nitric oxide fluorescent powder.
4. the method for preparing nitrogen oxide phosphor powder according to claim 1 is characterized in that: described reducing atmosphere is that 5% hydrogen and volumn concentration are that 95% nitrogen is formed by volumn concentration.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965107A (en) * | 2012-10-31 | 2013-03-13 | 彩虹集团公司 | Nitrogen oxide red fluorescent powder and preparation method thereof |
| CN103131414A (en) * | 2012-10-16 | 2013-06-05 | 彩虹集团公司 | Oxynitride yellow fluorescent powder and preparation method of the same |
| CN103525419A (en) * | 2013-09-27 | 2014-01-22 | 中国科学院长春应用化学研究所 | Method for preparing nitrogen oxygen silicate luminescent material in normal pressure and at low temperature |
| CN115305084A (en) * | 2022-07-20 | 2022-11-08 | 北京科技大学 | Aluminum oxynitride blue-cyan fluorescent powder excited by purple light, and preparation and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1861700A (en) * | 2006-05-26 | 2006-11-15 | 上海大学 | Preparation process of zirconium oxide base composite nano powder |
| CN101746813A (en) * | 2009-12-17 | 2010-06-23 | 昆明理工大学 | Preparation method of indium tin oxide nano-powder |
-
2010
- 2010-07-30 CN CN 201010241245 patent/CN101914379B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1861700A (en) * | 2006-05-26 | 2006-11-15 | 上海大学 | Preparation process of zirconium oxide base composite nano powder |
| CN101746813A (en) * | 2009-12-17 | 2010-06-23 | 昆明理工大学 | Preparation method of indium tin oxide nano-powder |
Non-Patent Citations (1)
| Title |
|---|
| 张梅 等: "白光LED用氮（氧）化合物荧光粉", 《化学进展》, vol. 22, no. 23, 30 April 2010 (2010-04-30), pages 377 - 382 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131414A (en) * | 2012-10-16 | 2013-06-05 | 彩虹集团公司 | Oxynitride yellow fluorescent powder and preparation method of the same |
| CN102965107A (en) * | 2012-10-31 | 2013-03-13 | 彩虹集团公司 | Nitrogen oxide red fluorescent powder and preparation method thereof |
| CN103525419A (en) * | 2013-09-27 | 2014-01-22 | 中国科学院长春应用化学研究所 | Method for preparing nitrogen oxygen silicate luminescent material in normal pressure and at low temperature |
| CN103525419B (en) * | 2013-09-27 | 2015-04-08 | 中国科学院长春应用化学研究所 | Method for preparing nitrogen oxygen silicate luminescent material in normal pressure and at low temperature |
| CN115305084A (en) * | 2022-07-20 | 2022-11-08 | 北京科技大学 | Aluminum oxynitride blue-cyan fluorescent powder excited by purple light, and preparation and application thereof |
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|---|---|
| CN101914379B (en) | 2013-06-19 |
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