CN1462789A - Red fluorescence powder - Google Patents
Red fluorescence powder Download PDFInfo
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- CN1462789A CN1462789A CN 03123790 CN03123790A CN1462789A CN 1462789 A CN1462789 A CN 1462789A CN 03123790 CN03123790 CN 03123790 CN 03123790 A CN03123790 A CN 03123790A CN 1462789 A CN1462789 A CN 1462789A
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Abstract
A red fluorescent powder in the form of sosoloid has a chemical formula: AxByC2-2y(MO4)2-(y-x)/2:2D, where A is chosen from Li, Na and K, B is chosen from Eu, Y, Gd and Lu, C is chosen from Mg, Ca and Sr, D is chosen from the fluorides of Ni, Na and K, M is Mo and/or W, x=0.1-1.0, y=0.4-1.0, and z=0-1.0. Its advantages are strong exciting absorption at near-ultraviolet band (370-410 nm), high light intensity and high color purity.
Description
Technical field
The present invention relates to a kind of fluorescent material of fluorescent-lamp-use, particularly a kind of molybdate is or/and tungstate red fluorescent powder.
Background technology
At present the luminescent lamp that uses mostly be utilize mercury vapor discharge produce wavelength be the ultraviolet ray of 254 nanometers as excitaton source, excitated fluorescent powder is luminous again, this class light source belongs to gas lamp.The shortcoming bulb volume of this class light source is big, and especially the calcium halophosphate activated by antimony andmanganese luminescent lamp will be used toxic materials mercury, and the life-span is short, and colour rendering index also remains further to be improved.Light source based on photodiode is the total solids light source, and its life-span is extremely long, and is pollution-free, and distant view luminous efficiency height, is called as the 21st century light source.Lumination of light emitting diode can be developed near ultraviolet at present, and wavelength is 370～410 nanometers, if mix the luminescent lamp of new generation that use then can obtain total solids with red-green-blue fluorescent material with this near ultraviolet photodiode.And present commercial fluorescent material is mostly developed at 254 nanometers and 365 nanometers of mercury, and near ultraviolet excitated fluorescent material seldom.Though wherein an applicant has submitted the patent application of " red fluorescence powder " to State Intellectual Property Office (application number has been 01138060.8 before this, the applying date is December 27 calendar year 2001, publication number is CN1357598A, open day is on July 10th, 2002), the document also discloses a kind of red fluorescence powder, and this red fluorescence powder has also closed MoO
3, Eu
2O
3, also contain one or more of oxide compound, fluorochemical of Ca, Sr, Cd, but do not relate to tungstate.And the disclosed fluorescent material of the document is not to be the near ultraviolet excitated of 370～410 nanometers at wavelength, neither be exclusively used in luminescent lamp, so it is that the near ultraviolet excitated effects such as luminous intensity of 370～410 nanometers also are not special ideals at wavelength.
Summary of the invention
At the deficiencies in the prior art, the object of the present invention is to provide a kind of molybdate of luminescent lamp that is used for or/and tungstate red fluorescent powder, this fluorescent material has the very strong absorption that excites, luminous intensity height, and high color purity at 370～410 nanometer near ultraviolet bands.
The object of the present invention is achieved like this.A kind of red fluorescence powder is sosoloid, and this sosoloid can be represented with following general formula:
A
xB
yC
2-2y(MO
4)
2-(y-x)/2：zD
Wherein A is one or more mixing uses of Li, Na, K, and when using for mixing, positively charged ion is pressed equivalence and substituted, and its molfraction summation is constant; B is that Eu, Y, one or more mixing of Gd, Lu are used, but Eu must be arranged, and when using for mixing, positively charged ion is pressed of equal value substituting, and its molfraction summation is constant; C is that one or more mixing of Mg, Ca, Sr are used, and when using for mixing, positively charged ion is pressed of equal value substituting, and its molfraction summation is constant; D is that one or more the mixing of LiF, NaF, KF is used, and when for mixing when using, its molfraction summation is constant; M is Mo or/and W, and when for mixing when using, its molfraction summation is constant;
In the above-mentioned sosoloid, 0.1≤x≤1.0,0.4＜y≤1.0,0≤z≤1.0, x≤y.
Above-mentioned sosoloid A
xB
yC
2-2y(MO
4)
2-(y-x)/2: the preferable range of x, z is among the zD: 0.4≤x≤1.0,0≤z≤0.50.
It is Li that above-mentioned sosoloid also can be preferably A, and B is Eu, and no C, D are LiF, y=1.0.
Prepare red fluorescence powder of the present invention and can promptly take by weighing following compounds: MoO in proportion with conventional high temperature solid phase synthesis
3Or/and WO
3, Eu
2O
3Or the carbonate of europium, oxalate, the carbonate of A is or/and one or more of fluorochemical mix use, the oxide compound of Y, Gd, Lu is or/and one or more of fluorochemical mix use, the carbonate of C or/and oxide compound or/and one or more of fluorochemical mix to use, after above-mentioned substance mixed, 500～1000 ℃ down reaction can obtain the sosoloid that need in 1～10 hour.
The present invention is with Eu
3+Be activator, technology is simple.Be mainly used in luminescent lamp, and fluorescent material disclosed in this invention have the very strong absorption that excites, luminous intensity height, high color purity at 370～410 nanometer near ultraviolet bands.
Description of drawings
Fig. 1 is the emmission spectrum figure of molybdate red phosphor;
Fig. 2 is the exciting light spectrogram of molybdate red phosphor;
Fig. 3 is the exciting light spectrogram of tungstate red fluorescent powder.
Embodiment
Further describe the present invention below by embodiment and accompanying drawing.
A kind of red fluorescence powder is sosoloid, and this sosoloid can be represented with following general formula:
A
xB
yC
2-2y(MO
4)
2-(y-x)/2：zD
Wherein A is one or more mixing uses of Li, Na, K, and when using for mixing, positively charged ion is pressed equivalence and substituted, and its molfraction summation is constant; B is that Eu, Y, one or more mixing of Gd, Lu are used, but Eu must be arranged, and when using for mixing, positively charged ion is pressed of equal value substituting, and its molfraction summation is constant; C is that one or more mixing of Mg, Ca, Sr are used, and when using for mixing, positively charged ion is pressed of equal value substituting, and its molfraction summation is constant; D is that one or more mixing of LiF, NaF, KF are used, and when using for mixing, its molfraction summation is constant; M is Mo or/and W, and when for mixing when using, its molfraction summation is constant;
In the above-mentioned sosoloid, 0.1≤x≤1.0,0.4＜y≤1.0,0≤z≤1.0, x≤y.
Above-mentioned sosoloid A
xB
yC
2-2y(MO
4)
2-(y-x)/2: the preferable range of x, z is among the zD: 0.4≤x≤1.0,0≤z≤0.5.
It is Li that above-mentioned sosoloid also can be preferably A, and B is Eu, and no C, D are LiF, y=1.0.
Prepare red fluorescence powder of the present invention and can promptly take by weighing following compounds: MoO in proportion with conventional high temperature solid phase synthesis
3Or/and WO
3, Eu
2O
3Or the carbonate of europium, oxalate, the carbonate of A is or/and the mixing use of one or more of fluorochemical, the oxide compound of Y, Gd, Lu is or/and the mixing use of one or more of fluorochemical, the carbonate of C or/and oxide compound or/and the mixing of one or more of fluorochemical use, after mix using above-mentioned substance evenly, 500～1000 ℃ down reaction can obtain the sosoloid that needs in 1～10 hour.
Embodiment 1: a kind of molybdate red phosphor is sosoloid A
xB
yC
2-2y(MoO
4)
2-(y-x)/2: zD, wherein A is Li, B is Eu, no C, no D, M are Mo, x=1.0, y=1.0, z=0, this sosoloid is for can be expressed as LiEuMo
2O
8, obtained in 3 hours by each component reaction under 800 degrees centigrade of following mol ratio:
MoO
3∶Eu
2O
3∶Li
2CO
3＝1.0∶0.25∶0.25
During preparation, MoO
3And Eu
2O
3The available salt that other can resolve into these oxide compounds substitutes, and finally is converted into oxide compound after the reaction and enters composition.Above-mentioned Li
2CO
3Also available corresponding organic acid salt or nitrate substitute.
Present embodiment is as the red fluorescence powder of fluorescent-lamp-use, its emmission spectrum figure such as Fig. 1, and its exciting light spectrogram such as Fig. 2, as can be seen from the figure, this fluorescent material has the very strong absorption that excites, luminous intensity height, high color purity at 370～410 nanometer near ultraviolet bands.
Embodiment 2: a kind of tungstate red fluorescent powder is sosoloid A
xB
yC
2-2y(WO
4)
2-(y-x)/2: zD, wherein A is Li, and B is Eu, and no C, D are LiF, and M is W, x=0.8, y=1.0, z=0.2, this sosoloid is for can be expressed as LiEuW
1.9O
7.6F
0.2, obtained in 4 hours by each component reaction under 950 degrees centigrade of following mol ratio:
WO
3∶Eu
2O
3∶Li
2CO
3∶LiF＝0.95∶0.25∶0.2∶0.1
During preparation, WO
3And Eu
2O
3The available salt that other can resolve into these oxide compounds substitutes, and finally is converted into oxide compound after the reaction and enters composition.Above-mentioned Li
2CO
3Also available corresponding organic acid salt or nitrate substitute.
Present embodiment is as the red fluorescence powder of fluorescent-lamp-use, and its emmission spectrum figure is similar to Fig. 1, its exciting light spectrogram such as Fig. 3, as can be seen from the figure, this fluorescent material has the very strong absorption that excites, luminous intensity height, high color purity at 370～410 nanometer near ultraviolet bands.
Embodiment 3: a kind of molybdenum tungstate red fluorescent powder is sosoloid A
xB
yC
2-2y(MO
4)
2-(y-x)/2: zD, wherein A is Li, and B is Eu, and no C, M are the mixing of Mo and W, and D is LiF, x=0.8, y=1.0, z=0.2, this sosoloid is for can be expressed as LiEuMo
0.7W
1.2O
7.6F
0.2, obtained in 4 hours by each component reaction under 850 degrees centigrade of following mol ratio:
MoO
3∶WO
3∶Eu
2O
3∶Li
2CO
3∶LiF＝0.35∶0.6∶0.25∶0.2∶0.1
During preparation, MoO
3, WO
3And Eu
2O
3The available salt that other can resolve into these oxide compounds substitutes, and finally is converted into oxide compound after the reaction and enters composition.Above-mentioned Li
2CO
3Also available corresponding organic acid salt or nitrate substitute.
Embodiment 4: a kind of molybdate red phosphor is sosoloid A
xB
yC
2-2y(MoO
4)
2-(y-x)/2: zD, wherein A is Li, and B is Eu, and C is Ca, and D is LiF, M is Mo, x=0.4, y=0.5, z=0.1, this sosoloid is for can be expressed as Li
0.5Eu
0.5CaMo
1.95O
7.8F
0.1, obtained in 4 hours by each component reaction under 750 degrees centigrade of following mol ratio:
MoO
3∶Eu
2O
3∶Li
2CO
3∶CaCO
3∶LiF＝0.975∶0.125∶0.1∶0.5∶0.05
During preparation, MoO
3And Eu
2O
3The available salt that other can resolve into these oxide compounds substitutes, and finally is converted into oxide compound after the reaction and enters composition.Above-mentioned Li
2CO
3Also available corresponding organic acid salt or nitrate substitute.
Embodiment 5: a kind of molybdate red phosphor is sosoloid A
xB
yC
2-2y(MoO
4)
2-(y-x)/2: zD, wherein A is Li, and B is Eu, and no C, D are LiF, and M is Mo, x=1.0, y=1.0, z=0.2, sosoloid can be expressed as Li
1.2EuMo
2O
8F
0.2, obtained in 5 hours by each component reaction under 700 degrees centigrade of following mol ratio:
MoO
3∶Eu
2O
3∶Li
2CO
3∶LiF＝1∶0.25∶0.25∶0.1
During preparation, MoO
3And Eu
2O
3The available salt that other can resolve into these oxide compounds substitutes, and finally is converted into oxide compound after the reaction and enters composition.Above-mentioned Li
2CO
3Also available corresponding organic acid salt or nitrate substitute.
Embodiment 6: a kind of molybdate red phosphor is sosoloid A
xB
yC
2-2y(MoO
4)
2-(y-x)/2: zD, wherein A is Li, and B is Eu, Lu, and no C, D are LiF, and M is Mo, x=1.0, y=1.0, z=0.1, sosoloid can be expressed as Li
1.1Eu
0.5Lu
0.5Mo
2O
8F
0.1, obtained in 2 hours by each component reaction under 850 degrees centigrade of following mol ratio:
MoO
3∶Eu
2O
3∶Li
2CO
3∶LiF∶Lu
2O
3＝1∶0.125∶0.25∶0.05∶0.125
During preparation, MoO
3And Eu
2O
3, Lu
2O
3The available salt that other can resolve into these oxide compounds substitutes, and finally is converted into oxide compound after the reaction and enters composition.Above-mentioned Li
2CO
3Also available corresponding organic acid salt or nitrate substitute.
Embodiment 7: a kind of molybdate red phosphor is sosoloid A
xB
yC
2-2y(MoO
4)
2-(y-x)/2: zD, wherein A is Li, and B is Eu, and no C, D are LiF, and M is Mo, x=0.2, y=1.0, z=1.0, sosoloid can be expressed as Li
1.2EuMo
1.6O
6.4F, descend reaction to obtain in 10 hours by each component of following mol ratio at 700 degrees centigrade:
MoO
3∶Eu
2O
3∶Li
2CO
3∶LiF＝0.8∶0.25∶0.05∶0.5
During preparation, MoO
3And Eu
2O
3The available salt that other can resolve into these oxide compounds substitutes, and finally is converted into oxide compound after the reaction and enters composition.Above-mentioned Li
2CO
3Also available corresponding organic acid salt or nitrate substitute.
Embodiment 8: a kind of molybdate red phosphor is sosoloid A
xB
yC
2-2y(MoO
4)
2-(y-x)/2: zD, wherein A is Li and Na, and B is Eu, and C is Ca and Sr, and D is LiF, M is Mo, x=0.4, y=0.6, z=0.2, sosoloid can be expressed as Li
0.4Na
0.2Eu
0.6Ca
0.6Sr
0.2Mo
1.9O
7.6F
0.2, obtained in 10 hours by each component reaction under 800 degrees centigrade of following mol ratio:
MoO
3∶Eu
2O
3∶Li
2CO
3∶Na
2CO
3∶CaCO
3∶SrCO
3∶LiF＝0.95∶0.15∶0.05∶0.05∶0.3∶0.1∶0.1
During preparation, MoO
3And Eu
2O
3The available salt that other can resolve into these oxide compounds substitutes, and finally is converted into oxide compound after the reaction and enters composition.Above-mentioned Li
2CO
3Also available corresponding organic acid salt or nitrate substitute.
Claims (11)
1. a red fluorescence powder is sosoloid, it is characterized in that: this sosoloid can be represented with following general formula
A
xB
yC
2-2y(MO
4)
2-(y-x)/2：zD
Wherein A is one or more mixing uses of Li, Na, K, and when using for mixing, positively charged ion is pressed equivalence and substituted, and its molfraction summation is constant; B is that Eu, Y, one or more mixing of Gd, Lu are used, but Eu must be arranged, and when using for mixing, positively charged ion is pressed of equal value substituting, and its molfraction summation is constant; C is that one or more mixing of Mg, Ca, Sr are used, and when using for mixing, positively charged ion is pressed of equal value substituting, and its molfraction summation is constant; D is that one or more mixing of LiF, NaF, KF are used, and when using for mixing, its molfraction summation is constant; M is Mo or/and W, and when for mixing when using, its molfraction summation is constant;
In the above-mentioned sosoloid, 0.1≤x≤1.0,0.4＜y≤1.0,0≤z≤1.0, x≤y.
2. a kind of red fluorescence powder according to claim 1 is characterized in that: sosoloid A
xB
yC
2-2y(MO
4)
2-(y-x)/2: 0.4≤x among the zD≤1.0,0≤z≤0.5.
3. a kind of red fluorescence powder according to claim 1 is characterized in that: A is Li in the sosoloid, and B is Eu, and no C, D are LiF, y=1.0.
4. according to claim 1,2 described a kind of red fluorescence powders, it is characterized by: A is Li, and B is Eu, no C, and no D, M are Mo, x=1.0, y=1.0, z=0, sosoloid are LiEuMo
2O
8
5. according to claim 1,2 described a kind of red fluorescence powders, it is characterized by: A is Li, and B is Eu, and no C, D are LiF, and M is W, x=0.8, and y=1.0, z=0.2, sosoloid are LiEuW
1.9O
7.6F
0.2
6. according to claim 1,2 described a kind of red fluorescence powders, it is characterized in that: A is Li, and B is Eu, and no C, D are LiF, and M is W and Mo, x=0.8, and y=1.0, z=0.2, M are Mo, sosoloid is LiEuMo
0.7W
1.2O
7.6F
0.2
7. according to claim 1,2 described a kind of red fluorescence powders, it is characterized by: A is Li, and B is Eu, and C is Ca, and D is LiF, and M is Mo, x=0.4, and y=0.5, z=0.1, M are Mo, sosoloid is Li
0.5Eu
0.5CaMo
1.95O
7.8F
0.1
8. according to claim 1,2 or 3 described a kind of red fluorescence powders, it is characterized by: A is Li, and B is Eu, and no C, D are LiF, and M is Mo, x=1.0, and y=1.0, z=0.2, M are Mo, sosoloid can be expressed as Li
1.2E μ Mo
2O
8F
0.2
9. according to claim 1,2 described a kind of red fluorescence powders, it is characterized by: A is Li, and B is Eu, Lu, and no C, D are LiF, and M is Mo, x=1.0, and y=1.0, z=0.1, M are Mo, sosoloid is Li
1.1Eu
0.5Lu
0.5Mo
2O
8F
0.1
10. according to claim 1,3 described a kind of red fluorescence powders, it is characterized by: A is Li, and B is Eu, and no C, D are LiF, and M is Mo, x=0.2, and y=1.0, z=1.0, M are Mo, sosoloid is Li
1.2EuMo
1.6O
6.4F.
11. according to claim 1,2 described a kind of red fluorescence powders, it is characterized by: A is Li and Na, B is Eu, and C is Ca and Sr, and D is LiF, and M is Mo, x=0.4, and y=0.6, z=0.2, sosoloid are Li
0.4Na
0.2Eu
0.6Ca
0.6Sr
0.2Mo
1.9O
7.6F
0.2
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03123790 CN1200071C (en) | 2003-05-21 | 2003-05-21 | Red fluorescence powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03123790 CN1200071C (en) | 2003-05-21 | 2003-05-21 | Red fluorescence powder |
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| Publication Number | Publication Date |
|---|---|
| CN1462789A true CN1462789A (en) | 2003-12-24 |
| CN1200071C CN1200071C (en) | 2005-05-04 |
Family
ID=29748374
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|---|---|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100503779C (en) * | 2005-01-05 | 2009-06-24 | 中国科学院长春光学精密机械与物理研究所 | Near ultraviolet fluorescent powder preparation method |
| CN100540629C (en) * | 2007-11-12 | 2009-09-16 | 中国科学院长春光学精密机械与物理研究所 | Near ultraviolet or blue-light excited red fluorescence powder and preparation method thereof |
| CN101168666B (en) * | 2006-11-30 | 2010-06-09 | 中国科学院长春光学精密机械与物理研究所 | Red phosphor powder used for white light LED and preparing method thereof |
| CN101255337B (en) * | 2008-03-13 | 2010-06-09 | 同济大学 | Preparation method of red-light fluorescent powder for LED or PDP display |
| CN102585831A (en) * | 2012-01-19 | 2012-07-18 | 苏州大学 | Europium-ion-excited fluoromolybdate red fluorescent powder and preparation method and application thereof |
| CN106520117A (en) * | 2016-10-31 | 2017-03-22 | 陕西科技大学 | A preparing method of LiLa(MoO4)2:Eu<3+> fluorescent powder |
| WO2022110747A1 (en) * | 2020-11-30 | 2022-06-02 | 华南理工大学 | Molybdate luminescent ceramic material for laser display, preparation method therefor and use thereof |
-
2003
- 2003-05-21 CN CN 03123790 patent/CN1200071C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100503779C (en) * | 2005-01-05 | 2009-06-24 | 中国科学院长春光学精密机械与物理研究所 | Near ultraviolet fluorescent powder preparation method |
| CN101168666B (en) * | 2006-11-30 | 2010-06-09 | 中国科学院长春光学精密机械与物理研究所 | Red phosphor powder used for white light LED and preparing method thereof |
| CN100540629C (en) * | 2007-11-12 | 2009-09-16 | 中国科学院长春光学精密机械与物理研究所 | Near ultraviolet or blue-light excited red fluorescence powder and preparation method thereof |
| CN101255337B (en) * | 2008-03-13 | 2010-06-09 | 同济大学 | Preparation method of red-light fluorescent powder for LED or PDP display |
| CN102585831A (en) * | 2012-01-19 | 2012-07-18 | 苏州大学 | Europium-ion-excited fluoromolybdate red fluorescent powder and preparation method and application thereof |
| CN106520117A (en) * | 2016-10-31 | 2017-03-22 | 陕西科技大学 | A preparing method of LiLa(MoO4)2:Eu<3+> fluorescent powder |
| WO2022110747A1 (en) * | 2020-11-30 | 2022-06-02 | 华南理工大学 | Molybdate luminescent ceramic material for laser display, preparation method therefor and use thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1200071C (en) | 2005-05-04 |
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