CN101962542A - Niobate-based red fluorescent powder for white LED as well as preparation method and application thereof - Google Patents
Niobate-based red fluorescent powder for white LED as well as preparation method and application thereof Download PDFInfo
- Publication number
- CN101962542A CN101962542A CN2010102813126A CN201010281312A CN101962542A CN 101962542 A CN101962542 A CN 101962542A CN 2010102813126 A CN2010102813126 A CN 2010102813126A CN 201010281312 A CN201010281312 A CN 201010281312A CN 101962542 A CN101962542 A CN 101962542A
- Authority
- CN
- China
- Prior art keywords
- preparation
- roasting
- fluorescent material
- led
- gram
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Luminescent Compositions (AREA)
Abstract
The invention discloses LED niobate-based red fluorescent powder, which is characterized in that the chemical general formula thereof is M(2-2x)Nb2O7:xEu<3+>, xA<+>, wherein M is one or more of Mg, Ca, Sr and Ba; A is one or more of Li, Na, K and Rb; and x is not less than 0.10 and less than 1.00. The preparation method of the LED niobate-based red fluorescent powder comprises the following steps: weighing the raw materials according to the molar ratio of M(2-2x)Nb2O7:xEu<3+>, xA<+>, grinding and mixing uniformly; (2) roasting the mixture of step (1) in a muffle furnace at a high temperature in the air atmosphere, wherein the roasting temperature is 1,000 to 1,600 DEG C and the roasting time is 3 to 15 h; and (3) performing post-treatment on the roasted product of the step (2). The fluorescent powder can be effectively activated by near ultraviolet and blue light to emit red light and can be perfectly matched with near ultraviolet and blue LED chips; moreover, the fluorescent powder has stable physical and chemical performance, does not react with oxygen, water, carbon dioxide and the like in the environment and is heat-resistant, nontoxic and environment-friendly; and the preparation method is simple and easy to operate, adopts direct roasting in the air and has good application prospect.
Description
Technical field
The invention belongs to rare earth luminescent material technical field, particularly red fluorescent powder for white radiation LED and its production and application.
Background technology
LED (light-emitting diode) is a kind of novel solid-state illumination electric light source, have that energy-efficient, environmental protection, overlong service life, volume are little, shock resistance, advantage such as luminescence response is fast and operating voltage is low, be used widely already in fields such as pilot lamp, signal lamps, white light LEDs has begun to initiate strong challenge to incandescent light, the luminescent lamp firm status in lighting field now now, be expected to progressively replace, thereby present huge market outlook.
White light LEDs produces white light and mainly contains two approach: first kind is with three kinds of LED combination results of red, green, blue white light; Second kind is to mix with LED de-excitation light conversion phosphor to form white light, this approach has two kinds of implementations, wherein mature methods is that blue-light LED chip and YAG:Ce yellow fluorescent powder are arranged in pairs or groups and realized white light emission (United States Patent (USP) 5998925), but owing to lack red light, the compound white light that obtains is cold white light, therefore, this scheme still need be added suitable red fluorescence powder and be improved its colour rendering index, another kind of scheme then is that red fluorescence powder plays a part very important with nearly purple LED chip (390-410nm) and red/green/blue three primary colors fluorescent powder combination.
The chip that is used for White-light LED illumination at present mainly is the near-ultraviolet light chip of 390-410nm and the blue chip about 465nm.And existing red fluorescence powder effectively excite the scope majority in shortwave UV zone, the launching efficiency under near ultraviolet and blue light is low.Therefore, near-ultraviolet light, the blue-ray LED of development efficient stable seem particularly important with red fluorescence powder.At present, still lack the red fluorescence powder that can be excited by near-ultraviolet light or blue-light LED chip of excellent performance on the market, especially can also be in conceptual phase by the rouge and powder that near-ultraviolet light LED and blue led excite.
At LED with in the report of red fluorescence powder, can luminous intensity and stable aspect all reach the also rarely found of application requiring.For example: the someone attempts Y
2O
2S:Eu
3+Be applied to the WLED field, yet, commercial at present red fluorescence powder Y
2O
2S:Eu
3+Have many shortcomings: luminous efficiency is low under near ultraviolet excitation, and the chemical property instability is decomposed easily, and the life-span is short, and separating out of element sulphur can cause corrosive effects to chip, thereby causes the inefficacy of entire device.The red fluorescence powder that main being expected of several classes that relates in document and patent report is used for LED also has: Ca
3(VO
4)
2: Eu
3+, YVO
4: Eu
3+, Y
2O
3: Eu
3+, Bi
3+, CaO:Eu
3+, CaMoO
4: Eu
3+, (Gd, Y, Eu)
2(MoO
4)
3: Sm
3+, (Sr, Ca) S:Eu
2+, Ca
5(SiO
4)
2Cl
2: Eu
2+, Sr
2Si
5N
8: Eu
2+Deng.The stable high-luminous-efficiency of wherein rare-earth activated oxynitride is good and come into one's own, as: Sr
2Si
5N
8: Eu
2+, SrSi
2O
2N
2: Eu
2+, need under high temperature (1600-1700 ℃) high nitrogen or ammonia pressure (10atm), finish but the matrix of this class material is synthetic, very harsh to the requirement of production unit.
At present about with Eu
3+Be active ions, niobate be the bibliographical information of red fluorescent powder for white radiation LED of matrix and patent seldom.Tae-Keun Park etc. has studied the Bi that mixes high density
3+To RNbO
4: Eu
3+(R=La, Y, the Gd) influence of photoluminescence performance (Joumal of the Korean Physical Society, 2008,52:431 ↑ 434); Zhou Liya etc. study Eu
3+Concentration is to LaNb
0.70V
0.30O
4: Eu
3+The influence of emmission spectrum, proved V
5+Mix make excitation band to long wave direction broadening (Joumal of Alloys and Compounds 2010,495:268-271).It is the LED fluorescent material of matrix that patent of invention CN1239673C and CN1331982C all relate to the niobate.
Summary of the invention
The purpose of this invention is to provide a kind of stable chemical performance, illumination effect is good, and ideal color purity can effectively be excited and the fluorescent material of burn red by near-ultraviolet light, blue-ray LED.
Another object of the present invention provides the preparation method of above-mentioned red fluorescence powder.The preparation method of this fluorescent material is simple, and easy handling is pollution-free, and cost is low.
A further object of the present invention is the application of fluorescent material of the present invention on white light LED electric light source.
For achieving the above object, the present invention is achieved through the following technical solutions:
Fluorescent material of the present invention adopts stable M
2-2xNb
2O
7Be matrix, adopt Eu
3+As active ions, with Li
+, Na
+, K
+Or Rb
+In one or more as the charge compensation ion, its chemical constitution general formula is M
2-2xNb
2O
7: xEu
3+, xA
+, wherein, M is one or more among Mg, Ca, Sr or the Ba; A is one or more among Li, Na, K or the Rb; 0.10≤x＜1.00.
The method for preparing fluorescent material that the present invention relates to is as follows:
(1) according to chemical constitution formula: M
2-2xNb
2O
7: xEu
3+, xA
+(wherein M is Mg, Ca, Sr, one or more among the Ba; A is Li, Na, K, a kind of or how several among the Rb; 0.10≤x＜1.00) the mol ratio of Yao Qiuing accurately takes by weighing raw material, grinds, and makes its mixing;
(2) mixture that step (1) is obtained is put into the high-temperature roasting of retort furnace air atmosphere, and the maturing temperature of mixture is 1000～1600 ℃, and roasting time is 5～12 hours;
(3) product of roasting that obtains in the step (2) is passed through last handling process again, promptly obtain this red fluorescence powder;
Raw material Nb of the present invention, Mg, Ca, Sr, Ba, Eu, Li, Na, K, Rb are simple substance, perhaps its oxide compound, perhaps its corresponding carbonate.
In the step of the present invention (1), can add reaction flux, described reaction flux is one or more in A halogenide, vitriol, boron trioxide or the boric acid.With respect to the gross weight of want synthetic fluorescent material, the add-on of fusing assistant is 0.001～10wt%.
In the step of the present invention (2), more than high-temperature roasting can be divided into once or twice; Each maturing temperature is 1000～1600 ℃, and roasting time is 3～15 hours.
In the step of the present invention (3), last handling process comprises fragmentation, comminution by gas stream, removal of impurities, oven dry and classification.Described removal of impurities process comprises pickling, alkali cleaning or washing.Described classification process comprises settling methods, method of sieving, hydraulic elutria-tion method or air classification method.
Application on white light LED electric light source of the present invention is to be prepared into electric light source with containing prepared fluorescent material of the present invention and near ultraviolet or blue-ray LED.
It is wide that institute of the present invention synthetic fluorescent material has excitation wavelength range, illumination effect is good, characteristics such as physical and chemical performance is stable, can effectively be excited and launch red light by near-ultraviolet light, blue light, thereby can be coated in and prepare novel white LED light source on the blue-ray LED, also can mate with near-ultraviolet light LED, the fluorescent material that mixes other colors, preparation white light or chromatic led light source show application prospects, and especially the application potential at the White-light LED illumination technical elements is huge.
Characteristics of the present invention:
(1) the present invention can make and can effectively be excited and the fluorescent material of the light that glows by near-ultraviolet light, blue light, and this powder can mate with near-ultraviolet light, blue-light LED chip well, is a kind of red fluorescent powder for white radiation LED of new high-efficiency.
(2) red fluorescence powder physical and chemical performance of the present invention is stable, does not react with oxygen in the environment, water, carbonic acid gas etc., and is heat-resisting, nontoxic, nuisanceless.
(3) red fluorescence powder, preparation method thereof of the present invention is simple and easy in operation, does not also use the special gas protection, and directly roasting in air has good application prospects.
Description of drawings
Fig. 1 is the Mg of embodiment 1 preparation
0.50Nb
2O
7:
0.75Eu
3+, 0.75Li
+Excitation spectrum (left side) under 608nm monitoring and the emmission spectrum (right side) of 395nm under exciting, as shown in the figure, this fluorescent material can effectively be excited by the ultraviolet of 220-490nm scope, near-ultraviolet light and blue light and to send ruddiness and purity of color that peak wavelength is positioned at about 608nm very high.
Fig. 2 is the Mg of embodiment 2 preparations
0.50Nb
2O
7:
0.75Eu
3+, 0.75Na
+Excitation spectrum (left side) under 608nm monitoring and the emmission spectrum (right side) of 395nm under exciting, as shown in the figure, this fluorescent material can effectively be excited by the ultraviolet of 220～490nm scope, near-ultraviolet light and blue light and to send ruddiness and purity of color that peak wavelength is positioned at about 608nm very high.
Fig. 3 is the Ca of embodiment 3 preparations
1.500Nb
2O
7:
0.375Eu
3+,
0.375Li
+Excitation spectrum (left side) under 608nm monitoring and the emmission spectrum (right side) under 395nm and 464nm excite respectively, as shown in the figure, this fluorescent material can effectively be excited by the near-ultraviolet light of 350-550nm scope, blue light and green glow and send peak wavelength and be positioned at ruddiness about 608nm, blue light has higher excitation intensity, and red purity is very high.
Fig. 4 is the Ca of embodiment 4 preparations
1.50Nb
2O
7:
0.25Eu
3+,
0.25Na
+Excitation spectrum (left side) under 608nm monitoring and the emmission spectrum (right side) under 395nm and 464nm excite respectively, as shown in the figure, this fluorescent material can effectively be excited by the near-ultraviolet light of 350-550nm scope, blue light and green glow and send peak wavelength and be positioned at ruddiness about 608nm, blue light has higher excitation intensity, and red purity is very high.
Fig. 5 is the Ca of embodiment 5 preparations
1.750Nb
2O
7:
0.125Eu
3+, 0.125K
+Excitation spectrum (left side) under 608nm monitoring and the emmission spectrum (right side) under 395nm and 464nm excite respectively, as shown in the figure, this fluorescent material can effectively be excited by the near-ultraviolet light of 350-550nm scope, blue light and green glow and send peak wavelength and be positioned at ruddiness about 608nm, blue light has higher excitation intensity, and red purity is very high.
Fig. 6 is the Sr of embodiment 6 preparations
1.75Nb
2O
7:
0.125Eu
3+,
0.125Li
+Excitation spectrum (left side) and the emmission spectrum under 464nm excites (right side) under 610nm monitoring, as shown in the figure, this fluorescent material can effectively be excited by the near-ultraviolet light of 350～550nm scope, blue light and green glow and send peak wavelength and be positioned at ruddiness about 610nm, blue light has higher excitation intensity, and red purity is very high.
Fig. 7 is the Sr of embodiment 7 preparations
1.25Nb
2O
7:
0.375Eu
3+,
0.375Na
+Excitation spectrum (left side) and the emmission spectrum under 464nm excites (right side) under 610nm monitoring, as shown in the figure, this fluorescent material can effectively be excited by the near-ultraviolet light of 350-550nm scope, blue light and green glow and send peak wavelength and be positioned at ruddiness about 610nm, blue light has higher excitation intensity, and red purity is very high.
Fig. 8 is the Sr of embodiment 8 preparations
1.75Nb
2O
7:
0.125Eu
3+,
0.125K
+Excitation spectrum (left side) and the emmission spectrum under 464nm excites (right side) under 610nm monitoring, as shown in the figure, this fluorescent material can effectively be excited by the near-ultraviolet light of 350～550nm scope, blue light and green glow and send peak wavelength and be positioned at ruddiness about 610nm, blue light has higher excitation intensity, and red purity is very high.
Fig. 9 is the BaNb of embodiment 9 preparations
2O
7:
0.50Eu
3+,
0.50Li
+Excitation spectrum (left side) and the emmission spectrum under 395nm excites (right side) under 612nm monitoring, as shown in the figure, this fluorescent material can effectively be excited by the near-ultraviolet light of 350～550nm scope, blue light and green glow and send peak wavelength and be positioned at high strength ruddiness about 612nm, wherein near-ultraviolet light has higher excitation intensity, and red purity is very high.
Figure 10 is the BaNb of embodiment 10 preparations
2O
7:
0.50Eu
3+,
0.50Na
+Excitation spectrum (left side) and the emmission spectrum under 395nm excites (right side) under 612nm monitoring, as shown in the figure, this fluorescent material can effectively be excited by the near-ultraviolet light of 350～550nm scope, blue light and green glow and send peak wavelength and be positioned at high strength ruddiness about 612nm, wherein near-ultraviolet light has higher excitation intensity, and red purity is very high.
Figure 11 is the Ba of embodiment 11 preparations
1.25Nb
2O
7:
0.375Eu
3+,
0.375K
+Excitation spectrum (left side) and the emmission spectrum under 395nm excites (right side) under 612nm monitoring, as shown in the figure, this fluorescent material can effectively be excited by the near-ultraviolet light of 350～550nm scope, blue light and green glow and send peak wavelength and be positioned at high strength ruddiness about 612nm, wherein near-ultraviolet light has higher excitation intensity, and red purity is very high.
Specific embodiments:
The present invention will be described further by following examples.
Embodiment 1:Mg
0.50Nb
2O
7:
0.75Eu
3+,
0.75Li
+The preparation embodiment of fluorescent material.
Take by weighing 0.4493 gram MgCO respectively
3(analytical pure), 2.8331 gram Nb
2O
5(99.999%), 1.4066 gram Eu
2O
3(99.999%) and 0.0040 the gram Li
2CO
3(analytical pure), in agate mortar ground and mixed evenly after, the alumina crucible of packing into, 1200 ℃ of roastings are 5 hours in air atmosphere, cool to room temperature with the furnace, and are levigate, promptly get the Mg among the present invention
0.50Nb
2O
7:
0.75Eu
3+,
0.75Li
+Red fluorescence powder.It excites with emmission spectrum sees Fig. 1.
Embodiment 2:Mg
1.50Nb
2O
7:
0.25Eu
3+,
0.25Na
+The preparation embodiment of fluorescent material.
Take by weighing 1.5129 gram MgCO respectively
3(analytical pure), 3.1798 gram Nb
2O
5(99.999%), 0.5262 gram Eu
2O
3(99.999%) and 0.1585 the gram Na
2CO
3(analytical pure), in agate mortar ground and mixed evenly after, the alumina crucible of packing into, 1200 ℃ of roastings are 5 hours in air atmosphere, cool to room temperature with the furnace, and are levigate, promptly get the Mg among the present invention
1.50Nb
2O
7:
0.25Eu
3+,
0.25Na
+Red fluorescence powder.It excites with emmission spectrum sees Fig. 2.
Embodiment 3:Ca
1.500Nb
2O
7:
0.375Eu
3+,
0.375Li
+The preparation embodiment of fluorescent material.
Take by weighing 1.3980 gram CaCO respectively
3(analytical pure), 2.9702 gram Nb
2O
5(99.999%), 0.7373 gram Eu
2O
3(99.999%) and 0.1548 the gram Li
2CO
3(analytical pure), in agate mortar ground and mixed evenly after, the alumina crucible of packing into, 1200 ℃ of roastings are 5 hours in air atmosphere, cool to room temperature with the furnace, and are levigate, promptly get the Ca among the present invention
1.500Nb
2O
7:
0.375Eu
3+,
0.375Li
+Red fluorescence powder.It excites with emmission spectrum sees Fig. 3.
Embodiment 4:Ca
1.50Nb
2O
7:
0.25Eu
3+,
0.25Na
+The preparation embodiment of fluorescent material.
Take by weighing 1.6997 gram CaCO respectively
3(analytical pure), 3.0094 gram Nb
2O
5(99.999%), 0.49804 gram Eu
2O
3(99.999%) and 0.1500 the gram Na
2CO
3(analytical pure), in agate mortar ground and mixed evenly after, the alumina crucible of packing into, 1200 ℃ of roastings are 5 hours in air atmosphere, cool to room temperature with the furnace, and are levigate, promptly get the Ca among the present invention
1.50Nb
2O
7:
0.25Eu
3+,
0.25Na
+Red fluorescence powder.It excites with emmission spectrum sees Fig. 4.
Embodiment 5:Ca
1.750Nb
2O
7:
0.125Eu
3+,
0.125K
+The preparation embodiment of fluorescent material.
Take by weighing 2.0282 gram CaCO respectively
3(analytical pure), 3.0780 gram Nb
2O
5(99.999%), 0.2547 gram Eu
2O
3(99.999%) and 0.1000 the gram K
2CO
3(analytical pure), in agate mortar ground and mixed evenly after, the alumina crucible of packing into, 1200 ℃ of roastings are 5 hours in air atmosphere, cool to room temperature with the furnace, and are levigate, promptly get the Ca among the present invention
1.750Nb
2O
7:
0.125Eu
3+,
0.125K
+Red fluorescence powder.It excites with emmission spectrum sees Fig. 5.
Embodiment 6:Sr
1.75Nb
2O
7:
0.125Eu
3+,
0.125Li
+The preparation embodiment of fluorescent material
Take by weighing 2.5280 gram SrCO respectively
3(analytical pure), 2.6010 gram Nb
2O
5(99.999%), 0.2152 gram Eu
2O
3(99.999%) and 0.0452 the gram Li
2CO
3(analytical pure), in agate mortar ground and mixed evenly after, the alumina crucible of packing into, 1200 ℃ of roastings are 5 hours in air atmosphere, cool to room temperature with the furnace, and are levigate, promptly get the Sr among the present invention
1.75Nb
2O
7:
0.125Eu
3+,
0.125Li
+Red fluorescence powder.It excites with emmission spectrum sees Fig. 6.
Embodiment 7:Sr
1.25Nb
2O
7:
0.375Eu
3+,
0.375Na
+The preparation embodiment of fluorescent material.
Take by weighing 1.7989 gram SrCO respectively
3(analytical pure), 2.5912 gram Nb
2O
5(99.999%), 0.6433 gram Eu
2O
3(99.999%) and 0.1937 the gram Na
2CO
3(analytical pure), in agate mortar ground and mixed evenly after, the alumina crucible of packing into, 1200 ℃ of roastings are 5 hours in air atmosphere, cool to room temperature with the furnace, and are levigate, promptly get the Sr among the present invention
1.25Nb
2O
7:
0.375Eu
3+,
0.375Na
+Red fluorescence powder.It excites with emmission spectrum sees Fig. 7.
Embodiment 8:Sr
1.75Nb
2O
7:
0.125Eu
3+,
0.125K
+The preparation embodiment of fluorescent material.
Take by weighing 2.5083 gram SrCO respectively
3(analytical pure), 2.5807 gram Nb
2O
5(99.999%), 0.2135 gram Eu
2O
3(99.999%) and 0.0839 the gram K
2CO
3(analytical pure), in agate mortar ground and mixed evenly after, the alumina crucible of packing into, 1200 ℃ of roastings are 5 hours in air atmosphere, cool to room temperature with the furnace, and are levigate, promptly get the Sr among the present invention
1.75Nb
2O
7:
0.125Eu
3+,
0.125K
+Red fluorescence powder.It excites with emmission spectrum sees Fig. 8.
Embodiment 9:BaNb
2O
7:
0.50Eu
3+,
0.50Li
+The preparation embodiment of fluorescent material.
Take by weighing 1.7792 gram BaCO respectively
3(analytical pure), 2.3966 gram Nb
2O
5(99.999%), 0.7933 gram Eu
2O
3(99.999%) and 0.1666 the gram Li
2CO
3(analytical pure), in agate mortar ground and mixed evenly after, the alumina crucible of packing into, 1200 ℃ of roastings are 5 hours in air atmosphere, cool to room temperature with the furnace, and are levigate, promptly get the BaNb among the present invention
2O
7:
0.50Eu
3+,
0.50Li
+Red fluorescence powder.It excites with emmission spectrum sees Fig. 9.
Embodiment 10:BaNb
2O
7:
0.50Eu
3+,
0.50Na
+The preparation embodiment of fluorescent material.
Take by weighing 1.7538 gram BaCO respectively
3(analytical pure), 2.3624 gram Nb
2O
5(99.999%), 0.7819 gram Eu
2O
3(99.999%) and 0.2355 the gram Li
2CO
3(analytical pure), in agate mortar ground and mixed evenly after, the alumina crucible of packing into, 1200 ℃ of roastings are 5 hours in air atmosphere, cool to room temperature with the furnace, and are levigate, promptly get the BaNb among the present invention
2O
7:
0.50Eu
3+,
0.50Na
+Red fluorescence powder.It excites with emmission spectrum sees Figure 10.
Embodiment 11:Ba
1.25Nb
2O
7:
0.375Eu
3+,
0.375K
+The preparation embodiment of fluorescent material.
Take by weighing 2.1225 gram BaCO respectively
3(analytical pure), 2.2872 gram Nb
2O
5(99.999%), 0.5678 gram Eu
2O
3(99.999%) and 0.2230 the gram Li
2CO
3(analytical pure), in agate mortar ground and mixed evenly after, the alumina crucible of packing into, 1200 ℃ of roastings are 5 hours in air atmosphere, cool to room temperature with the furnace, and are levigate, promptly get the Ba among the present invention
1.25Nb
2O
7:
0.375Eu
3+,
0.375K
+Red fluorescence powder.It excites with emmission spectrum sees Figure 11.
Claims (8)
1. LED niobate red fluorescence powder is characterized in that its chemical constitution general formula is:
M
2-2xNb
2O
7:xEu
3+，xA
+
Wherein, M is one or more among Mg, Ca, Sr or the Ba; A is one or more among Li, Na, K or the Rb; 0.10≤x＜1.00.
2. the preparation method of the described fluorescent material of claim 1 is characterized in that:
(1) according to chemical constitution formula: M
2-2xNb
2O
7: xEu
3+, xA
+Mol ratio, take by weighing raw material, grind mixing;
(2) mixture that step (1) is obtained is put into the high-temperature roasting of retort furnace air atmosphere, and the maturing temperature of mixture is 1000-1600 ℃, and roasting time is 3～15 hours;
(3) product of roasting that obtains in the step (2) is passed through last handling process again, promptly obtain this red fluorescence powder.
3. preparation method according to claim 2 is characterized in that described raw material Nb, Mg, Ca, Sr, Ba, Eu, Li, Na, K, Rb are simple substance, perhaps its oxide compound, perhaps its corresponding salt.
4. preparation method according to claim 2 is characterized in that in described step (1), adds reaction flux, and reaction flux is one or more in A halogenide, vitriol, boron trioxide or the boric acid.
5. preparation method according to claim 4 is characterized in that the gross weight with respect to want synthetic fluorescent material, and the add-on of fusing assistant is 0.001～10wt%.
6. preparation method according to claim 2 is characterized in that in the described step (2), more than high-temperature roasting is divided into once or twice; Each maturing temperature is 1000～1600 ℃, and roasting time is 3～15 hours.
7. preparation method according to claim 2 is characterized in that last handling process comprises fragmentation, comminution by gas stream, removal of impurities in the described step (3), oven dry and classification.
8. the application of the described fluorescent material of claim 1 is characterized in that being prepared into electric light source with containing described fluorescent material of claim 1 and near ultraviolet or blue-ray LED.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010281312 CN101962542B (en) | 2010-09-14 | 2010-09-14 | Niobate-based red fluorescent powder for white LED as well as preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010281312 CN101962542B (en) | 2010-09-14 | 2010-09-14 | Niobate-based red fluorescent powder for white LED as well as preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101962542A true CN101962542A (en) | 2011-02-02 |
| CN101962542B CN101962542B (en) | 2013-06-05 |
Family
ID=43515598
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010281312 Expired - Fee Related CN101962542B (en) | 2010-09-14 | 2010-09-14 | Niobate-based red fluorescent powder for white LED as well as preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101962542B (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899299A (en) * | 2010-06-25 | 2010-12-01 | 海洋王照明科技股份有限公司 | Niobate luminescent material and preparation method thereof |
| CN102250616A (en) * | 2011-05-06 | 2011-11-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | Double-perovskite structured red fluorescent powder as well as preparation method and application thereof |
| CN103992795A (en) * | 2014-05-05 | 2014-08-20 | 青岛大学 | Red phosphor for LED, and preparation method thereof |
| CN104560040A (en) * | 2015-01-23 | 2015-04-29 | 南京工业大学 | Niobate fluorescent powder for near ultraviolet white light LED and preparation method thereof |
| CN105524615A (en) * | 2015-12-14 | 2016-04-27 | 常熟理工学院 | Niobate red phosphor for white-light LEDs and preparation method thereof |
| CN105694886A (en) * | 2015-12-23 | 2016-06-22 | 江苏师范大学 | Eu (Eu)2+Preparation method and application of doped fluosilicate-based luminescent material |
| CN105732033A (en) * | 2016-03-16 | 2016-07-06 | 武汉理工大学 | Barium magnesium niobate light-emitting ceramics and preparation method thereof |
| CN105778908A (en) * | 2016-04-06 | 2016-07-20 | 青岛大学 | Calcium-niobate-based self-activated light emitting material, preparation method and application |
| CN105860971A (en) * | 2016-04-22 | 2016-08-17 | 江苏师范大学 | Rare earth ion doped zirconium niobate fluorescent powder and preparation method thereof |
| CN108893112A (en) * | 2018-08-09 | 2018-11-27 | 中山大学 | A kind of red fluorescence powder and preparation method thereof that the trivalent europium ion applied to WLED device adulterates |
| CN111363545A (en) * | 2020-04-22 | 2020-07-03 | 吉林大学 | Eu (Eu)3+Preparation method and application of pyrochlore-doped luminescent material |
| CN116814263A (en) * | 2023-06-07 | 2023-09-29 | 云南大学 | Single-phase white light fluorescent material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1597097A (en) * | 2004-08-30 | 2005-03-23 | 南京大学 | Preparation method of high specific surface tantalate and niobate photo catalyst |
| CN101174756A (en) * | 2007-11-30 | 2008-05-07 | 中国科学院上海光学精密机械研究所 | Ytterbium-doped calcium niobate laser crystal and preparation method thereof |
-
2010
- 2010-09-14 CN CN 201010281312 patent/CN101962542B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1597097A (en) * | 2004-08-30 | 2005-03-23 | 南京大学 | Preparation method of high specific surface tantalate and niobate photo catalyst |
| CN101174756A (en) * | 2007-11-30 | 2008-05-07 | 中国科学院上海光学精密机械研究所 | Ytterbium-doped calcium niobate laser crystal and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 《Materials Research Bulletin》 19991231 Brian L. Cushing et. al. A TWO-STEP ION EXCHANGE ROUTE TO THE NEW METASTABLE DOUBLE-LAYERED PEROVSKITE,(Rb,Na)1-xCax/2LaNb2O7(X≈0.9) 第271-278页 1-8 第34卷, 第2期 * |
| BRIAN L. CUSHING ET. AL.: "A TWO-STEP ION EXCHANGE ROUTE TO THE NEW METASTABLE DOUBLE-LAYERED PEROVSKITE,(Rb,Na)1-xCax/2LaNb2O7(X≈0.9)", 《MATERIALS RESEARCH BULLETIN》 * |
| N. FLOROS ET. AL.: "New n=2 members of the Li2Srn-1MnO3n+1 family, closely related to the Ruddlesden-Popper phases: structure and non-stoichiometry", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899299A (en) * | 2010-06-25 | 2010-12-01 | 海洋王照明科技股份有限公司 | Niobate luminescent material and preparation method thereof |
| CN101899299B (en) * | 2010-06-25 | 2013-11-27 | 海洋王照明科技股份有限公司 | Niobate luminescent material and preparation method thereof |
| CN102250616A (en) * | 2011-05-06 | 2011-11-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | Double-perovskite structured red fluorescent powder as well as preparation method and application thereof |
| CN102250616B (en) * | 2011-05-06 | 2014-01-01 | 中国科学院苏州纳米技术与纳米仿生研究所 | Double-perovskite structured red fluorescent powder as well as preparation method and application thereof |
| CN103992795A (en) * | 2014-05-05 | 2014-08-20 | 青岛大学 | Red phosphor for LED, and preparation method thereof |
| CN103992795B (en) * | 2014-05-05 | 2016-04-06 | 青岛大学 | A kind of LED red fluorescence powder and preparation method thereof |
| CN104560040A (en) * | 2015-01-23 | 2015-04-29 | 南京工业大学 | Niobate fluorescent powder for near ultraviolet white light LED and preparation method thereof |
| CN105524615A (en) * | 2015-12-14 | 2016-04-27 | 常熟理工学院 | Niobate red phosphor for white-light LEDs and preparation method thereof |
| CN105694886A (en) * | 2015-12-23 | 2016-06-22 | 江苏师范大学 | Eu (Eu)2+Preparation method and application of doped fluosilicate-based luminescent material |
| CN105732033A (en) * | 2016-03-16 | 2016-07-06 | 武汉理工大学 | Barium magnesium niobate light-emitting ceramics and preparation method thereof |
| CN105778908A (en) * | 2016-04-06 | 2016-07-20 | 青岛大学 | Calcium-niobate-based self-activated light emitting material, preparation method and application |
| CN105860971A (en) * | 2016-04-22 | 2016-08-17 | 江苏师范大学 | Rare earth ion doped zirconium niobate fluorescent powder and preparation method thereof |
| CN105860971B (en) * | 2016-04-22 | 2018-04-20 | 江苏师范大学 | Rare earth ion doped zirconium niobate fluorescent powder and preparation method thereof |
| CN108893112A (en) * | 2018-08-09 | 2018-11-27 | 中山大学 | A kind of red fluorescence powder and preparation method thereof that the trivalent europium ion applied to WLED device adulterates |
| CN111363545A (en) * | 2020-04-22 | 2020-07-03 | 吉林大学 | Eu (Eu)3+Preparation method and application of pyrochlore-doped luminescent material |
| CN116814263A (en) * | 2023-06-07 | 2023-09-29 | 云南大学 | Single-phase white light fluorescent material and preparation method and application thereof |
| CN116814263B (en) * | 2023-06-07 | 2024-05-28 | 云南大学 | Single-phase white light fluorescent material and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101962542B (en) | 2013-06-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101962542B (en) | Niobate-based red fluorescent powder for white LED as well as preparation method and application thereof | |
| CN101475802B (en) | Multiple antimonate luminescent materials for white light LED and preparation thereof | |
| CN102533266A (en) | Europium-activated tungsten molybdate red fluorescent powder for white LED (Light Emitting Diode) and preparation method of europium-activated tungsten molybdate red fluorescent powder | |
| CN105331364A (en) | YAG:Mn red phosphor, preparation method and applications thereof | |
| CN101851508A (en) | Europium activated silicate green fluorescent powder and application thereof in white light emitting diode | |
| CN101402857B (en) | Red luminous material for LED and producing process thereof | |
| CN102492423A (en) | Red fluorescent material used for white LED (light-emitting diode) and preparation method thereof | |
| CN105349147A (en) | Ultraviolet-to-blue light excited phosphate-based red fluorescent powder and preparation method thereof | |
| CN103059849B (en) | Silicophosphate green fluorescent powder activated by Eu<2+> and preparation method as well as application thereof | |
| CN104987864A (en) | Layered perovskite red phosphor for white LED and preparation method thereof | |
| CN103275713A (en) | Rare earth molybdate red phosphor, and preparation method and application thereof | |
| CN103305216A (en) | Borate red fluorescent powder and preparation method and application thereof | |
| CN102433119A (en) | Tungsten molybdate red fluorescent powder for white light LED and preparation method thereof | |
| CN105368450A (en) | Double-perovskite tungstate white light phosphor and preparation method thereof | |
| CN102838989B (en) | Ultraviolet excited borate-based white fluorescent powder and preparation method thereof | |
| CN102604633A (en) | Tetratungstate red phosphor powder and preparation method thereof | |
| CN101760191B (en) | High-brightness barium-silicate-based blue-green fluorescent powder for LED and high-temperature reducing preparation method thereof | |
| CN103694999A (en) | Europium ion activated phosphate red fluorescent powder and preparation method thereof | |
| CN103952151A (en) | Europium ion activated silicon phosphate green fluorescent powder and its preparation method | |
| CN102492422A (en) | Green emitting phosphor for white-light LEDs and preparation method thereof | |
| CN101987957B (en) | Red phosphor powder for white LED as well as preparation method and application thereof | |
| CN102002362B (en) | Fluorescent powder for white light LED, preparation method and application thereof | |
| CN101982520A (en) | Rare earth phosphor red luminous material for converting purple light emitting diode (LED) to white light LED and preparation method thereof | |
| CN105838369B (en) | A kind of orange red fluorescent powder and preparation method thereof | |
| CN103320127A (en) | Borate-based red fluorescent powder used for white light LED and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130605 Termination date: 20180914 |