CN103087709A - Cerium-ion-doped silicate blue fluorescent powder and preparation method thereof - Google Patents
Cerium-ion-doped silicate blue fluorescent powder and preparation method thereof Download PDFInfo
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- CN103087709A CN103087709A CN2013100279655A CN201310027965A CN103087709A CN 103087709 A CN103087709 A CN 103087709A CN 2013100279655 A CN2013100279655 A CN 2013100279655A CN 201310027965 A CN201310027965 A CN 201310027965A CN 103087709 A CN103087709 A CN 103087709A
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Abstract
The invention provides cerium-ion-doped silicate blue fluorescent powder and a preparation method thereof. The chemical formula of the cerium-ion-doped silicate blue fluorescent powder is Sr2-xMgSi2O7:xCe<3+>, wherein x is more than or equal to 0.0001 and less than or equal to 0.3; and the preparation method comprises the following steps of: 1) weighing a compound containing Sr, a compound containing Mg, a compound containing Si and a compound containing Ce, mixing and then grinding for 30-60 minutes; 2) drying the ground mixed powder and continuously grinding to form powder; 3) carrying out high-temperature calcining for 2-48 hours in reducing atmosphere; and 4) crushing and grinding the calcined powder, and grading to obtain the cerium-ion-doped silicate blue fluorescent powder. The blue fluorescent powder prepared by the invention is good in crystal development and wider in emission spectrum and can better meet the packaging requirement of a white LED (light-emitting diode), chromaticity and luminosity stability are better, raw materials are cheap and easy to get, the preparation method is simple and practicable, and industrial production can be realized.
Description
Technical field
The present invention relates to luminescent material, particularly a kind of cerium ion-doped silicate blue fluorescent powder and preparation method thereof.
Background technology
White light LEDs (White Light Emitting Diodes, WLED) is as a kind of novel solid light source, and, environmental protection energy-conservation with it, the plurality of advantages such as the life-span is long and volume is little have huge application prospect in illumination and demonstration field.At present, utilize the LED technology to realize that the mode of white light has 3 kinds: (1) blue chip excites gold-tinted and the remaining blue light that yellow fluorescent powder sends to be combined into white light; (2) utilize the near ultraviolet LED chip to excite the red, green, blue three primary colors fluorescent powder and organically combine the composition white light; (3) assemble together by red light chips, green glow chip and blue chip and realize white light.At present, the first form is the main flow form of synthesize white light, but requires at 420～470nm based on the absorption peak of the light-converting material of blue-ray LED, and the fluorescent material that can satisfy this requirement is considerably less.Because yellow fluorescent powder lacks the ruddiness composition, colour rendering index is low, and the glow color of device changes with the variation of driving voltage and fluorescent coating thickness, and color reducibility is poor.For addressing the above problem, adopt near-ultraviolet light InGaN tube core to excite three primary colors fluorescent powder to realize that white light LEDs is a kind of replacement scheme preferably.The white light LEDs that this mode obtains, the excitation energy of its chip is higher than blue chip, therefore can improve the fluorescent material launching efficiency.Because near-ultraviolet light is invisible to naked eyes, the color of this class white light LEDs is only determined by fluorescent material.The three primary colors fluorescent powder white light LEDs is compared with the yellow YAG fluorescent material of InGaN blue-light LED chip conversion hysteria, the stability of colourity and luminosity aspect is better, the emmission spectrum of its fluorescent material is wider, more near the spectrum of nature white light, colour rendering index is high, chromaticity coordinates is affected less.
At present, the near ultraviolet LED blue colour fluorescent powder is mainly BaMgAl10O17:Eu
2+(BAM), but BAM is very weak in the absorption at 400nm place, can not mate with the InGaN chip well, and synthesis temperature is higher, fluorescent material easily lumps under the synthesis temperature of 1300 ℃, and the blue colour fluorescent powder that therefore is necessary to develop a kind of novel near ultraviolet excitation substitutes the BAM of commercialization at present.Ce
3+Be a kind of important activator, have the 4f15d0 electronic configuration, its 4f1 electronics can be energized into the lower 5d attitude of energy. can realize luminous in very wide spectral range.With respect to the fluorescent material of other matrix, it is cheap and easy to get that silicate systems fluorescent material has raw material, and chemical stability and thermostability are higher, the phototransformation rate is high, crystal property and light transmission are excellent, have the wide range excitation band, and emmission spectrum is the series of advantages such as adjustable continuously.Therefore, rare-earth ion activated silicate-base fluorescent material is regarded as a kind of up-and-coming luminescent material.
Summary of the invention
The object of the present invention is to provide a kind of cerium ion-doped silicate blue fluorescent powder and preparation method thereof, the fluorescent material emmission spectrum is wider, more near the spectrum of nature white light, and colourity and luminosity stability are better, and with low cost, preparation technology is simple, and crystal property is good.
The present invention is by the following technical solutions for achieving the above object:
A kind of cerium ion-doped silicate blue fluorescent powder, chemical formula are Sr2-xMgSi2O7:xCe3+, and wherein x is 0.0001≤x≤0.3.
A kind of preparation method of cerium ion-doped silicate blue fluorescent powder comprises the following steps:
1) according to Sr2-xMgSi2O7:xCe3+, wherein x is the stoichiometric ratio of each element in 0.0001≤x≤0.3, and weighing contains the compound of Sr, contains the compound of Mg, contains the compound of Si, contains the compound of Ce, grinds 30 ~ 60min after mixing;
2) continue the shape of pulverizing after the mixed powder drying after grinding;
3) will be through step 2) mixed powder after grinding is placed in crucible, and high-temperature roasting 2 ~ 48h in reducing atmosphere, maturing temperature are 1100 ~ 1300 ℃;
4) the powder crushing grinding after calcining, classification obtains cerium ion-doped silicate blue fluorescent powder.
Step 1) will contain the compound of Sr, contain the compound of Mg, contain the compound of Si, and the compound and the boric acid that contain Ce are placed in agate mortar, add alcohol to mix the rear 30 ~ 60min of grinding, and described boric acid is 0.01 ~ 0.1:1 with the mol ratio that contains the compound of Sr.
The described compound that contains Sr contains the compound of Mg, contains the compound of Si, and the compound and the boric acid that contain Ce are analytical pure.
The compound of the described Sr of containing is Strontium carbonate powder SrCO
3Or strontium nitrate Sr (NO
3)
2Or mixture both, the compound that contains Mg is magnesium oxide MgO or magnesium hydroxide Mg (OH)
2Or mixture both, the compound that contains Si is silicon-dioxide SiO
2Or water glass Na
2SiO
3Or mixture both, the compound that contains Ce is cerium oxide CeO
2Or cerous nitrate Ce (NO
3)
3Or mixture both.
Described reducing atmosphere is provided by the mixed gas of gac or hydrogen and nitrogen.
The present invention has following beneficial effect:
1) Sr2-xMgSi2O7:xCe of the present invention's preparation
3+The blue colour fluorescent powder crystal development is good, at ultraviolet/near-ultraviolet light (very strong blue light of emission under 320 ~ 410nm) exciting, it is wider that its emission peak is positioned at 380 ~ 480nm emmission spectrum, the fluorescence spectrum halfwidth is 45 ~ 75nm, can satisfy preferably the encapsulation requirement of white light LEDs, colourity and luminosity stability are better.
2) Sr of the present invention's preparation
2-xMgSi
2O
7: xCe
3+The blue-fluorescence powder raw material is cheap and easy to get, and the preparation method is simple, can realize suitability for industrialized production.
Description of drawings
The Sr of Fig. 1 the present invention preparation
2-xMgSi
2O
7: xCe
3+The XRD figure of blue colour fluorescent powder.
The Sr of Fig. 2 the present invention preparation
2-xMgSi
2O
7: xCe
3+The utilizing emitted light spectrogram of blue colour fluorescent powder.
Embodiment
The invention will be further described below in conjunction with concrete embodiment:
Embodiment 1:
According to Sr
1.9999MgSi
2O
7: 0.0001Ce
3+In the stoichiometric ratio of each element, the analytically pure SrCO of accurate weighing
3, MgO, SiO
2, CeO
2And H
3BO
3Be placed in agate mortar, add a small amount of alcohol and grind 30 ~ 60min, H
3BO
3With SrCO
3Mol ratio be 0.03:1, continue to grind 10min after oven dry at 60 ~ 120 ℃ of temperature, then be placed in 1100 ℃ of insulation 48h of crucible, waiting temperature drops to that to take out product after room temperature broken, grinds, classification can obtain the blue colour fluorescent powder that will prepare.
Embodiment 2:
According to Sr
1.99MgSi
2O
7: 0.01Ce
3+In the stoichiometric ratio of each element, the analytically pure SrCO of accurate weighing
3, MgO, SiO
2, CeO
2And H
3BO
3Be placed in agate mortar, add a small amount of alcohol and grind 30 ~ 60min, H
3BO
3With SrCO
3Mol ratio be 0.01:1, continue to grind 10min after oven dry at 60 ~ 120 ℃ of temperature, then be placed in 1200 ℃ of insulation 24h of crucible, waiting temperature drops to that to take out product after room temperature broken, grinds, classification can obtain the blue colour fluorescent powder that will prepare.
Embodiment 3:
According to Sr
1.97MgSi
2O
7: 0.03Ce
3+In the stoichiometric ratio of each element, the analytically pure SrCO of accurate weighing
3, MgO, SiO
2, CeO
2And H
3BO
3Be placed in agate mortar, add a small amount of alcohol and grind 30 ~ 60min, H
3BO
3With SrCO
3Mol ratio be 0.05:1, continue to grind 10min after oven dry at 60 ~ 120 ℃ of temperature, then be placed in 1250 ℃ of insulation 12h of crucible, waiting temperature drops to that to take out product after room temperature broken, grinds, classification can obtain the blue colour fluorescent powder that will prepare.
Embodiment 4:
According to Sr
1.9999MgSi
2O
7: 0.0001Ce
3+In the stoichiometric ratio of each element, the analytically pure SrCO of accurate weighing
3, MgO, SiO
2, CeO
2And H
3BO
3Be placed in agate mortar, add a small amount of alcohol and grind 30 ~ 60min, H
3BO
3With SrCO
3Mol ratio be 0.08:1, continue to grind 10min after oven dry at 60 ~ 120 ℃ of temperature, then be placed in 1250 ℃ of insulation 30h of crucible, waiting temperature drops to that to take out product after room temperature broken, grinds, classification can obtain the blue colour fluorescent powder that will prepare.
Embodiment 5:
According to Sr
1.7MgSi
2O
7: 0.3Ce
3+In the stoichiometric ratio of each element, the analytically pure SrCO of accurate weighing
3, MgO, SiO
2, CeO
2And H
3BO
3Be placed in agate mortar, add a small amount of alcohol and grind 30 ~ 60min, H
3BO
3With SrCO
3Mol ratio be 0.1:1, continue to grind 10min after oven dry at 60 ~ 120 ℃ of temperature, then be placed in 1300 ℃ of insulation 10h of crucible, waiting temperature drops to that to take out product after room temperature broken, grinds, classification can obtain the blue colour fluorescent powder that will prepare.
Embodiment 6: according to Sr
1.7MgSi
2O
7: 0.2Ce
3+In the stoichiometric ratio of each element, the analytically pure Sr (NO of accurate weighing
3)
2, Mg (OH)
2, Na
2SiO
3, Ce (NO
3)
3And H
3BO
3Be placed in agate mortar, add a small amount of alcohol and grind 30 ~ 60min, H
3BO
3With Sr (NO
3)
2Mol ratio be 0.1:1, continue to grind 10min after oven dry at 60 ~ 120 ℃ of temperature, then be placed in 1300 ℃ of insulation 2h of crucible, waiting temperature drops to that to take out product after room temperature broken, grinds, classification can obtain the blue colour fluorescent powder that will prepare.
Embodiment 7: according to Sr
1.7MgSi
2O
7: 0.02Ce
3+In the stoichiometric ratio of each element, the analytically pure Sr (NO of accurate weighing
3)
2And SrCO
3Mixture, Mg (OH)
2Mixture, Na with MgO
2SiO
3And SiO
2Mixture, Ce (NO
3)
3And CeO
2Mixture, with H
3BO
3Be placed in agate mortar, add a small amount of alcohol and grind 30 ~ 60min, H
3BO
3With Sr (NO
3)
2And SrCO
3The mol ratio of mixture is 0.1:1, and rear continuation of oven dry ground 10min at 60 ~ 120 ℃ of temperature, then is placed in 1200 ℃ of insulation 2h of crucible, and waiting temperature takes out the product fragmentation after dropping to room temperature, grinds, and classification can obtain the blue colour fluorescent powder that will prepare.
With reference to figure 1 and Fig. 2, the Sr of the present invention preparation as seen from Figure 1
2-xMgSi
2O
7: xCe
3+The blue colour fluorescent powder crystal property is good, and phase purity is high.The Sr of the present invention preparation as seen from Figure 2
2-xMgSi
2O
7: xCe
3+It is wider that its emission peak of blue colour fluorescent powder is positioned at 380 ~ 480nm emmission spectrum, can satisfy preferably the encapsulation requirement of white light LEDs.
Claims (6)
1. a cerium ion-doped silicate blue fluorescent powder, is characterized in that; Chemical formula is Sr
2-xMgSi
2O7
:xCe
3+, wherein x is 0.0001≤x≤0.3.
2. the preparation method of a cerium ion-doped silicate blue fluorescent powder, is characterized in that, comprises the following steps:
1) according to Sr
2-xMgSi
2O
7: xCe
3+, wherein x is the stoichiometric ratio of each element in 0.0001≤x≤0.3, weighing contains the compound of Sr, contains the compound of Mg, contains the compound of Si, contains the compound of Ce, grinds 30 ~ 60min after mixing;
2) continue the shape of pulverizing after the mixed powder drying after grinding;
3) will be through step 2) mixed powder after grinding is placed in crucible, and high-temperature roasting 2 ~ 48h in reducing atmosphere, maturing temperature are 1100 ~ 1300 ℃;
4) the powder crushing grinding after calcining, classification obtains cerium ion-doped silicate blue fluorescent powder.
3. the preparation method of a kind of cerium ion-doped silicate blue fluorescent powder according to claim 2, it is characterized in that: step 1) will contain the compound of Sr, the compound that contains Mg, the compound that contains Si, the compound and the boric acid that contain Ce are placed in agate mortar, grind 30 ~ 60min after adding alcohol to mix, described boric acid is 0.01 ~ 0.1: 1 with the mol ratio that contains the compound of Sr.
4. the preparation method of a kind of cerium ion-doped silicate blue fluorescent powder according to claim 3 is characterized in that: the compound of the described Sr of containing, contain the compound of Mg, and contain the compound of Si, the compound and the boric acid that contain Ce are analytical pure.
5. the preparation method of a kind of cerium ion-doped silicate blue fluorescent powder according to claim 2, it is characterized in that: the compound of the described Sr of containing is Strontium carbonate powder SrCO
3Or strontium nitrate Sr (NO
3)
2Or mixture both, the compound that contains Mg is magnesium oxide MgO or magnesium hydroxide Mg (OH)
2Or mixture both, the compound that contains Si is silicon-dioxide SiO
2Or water glass Na
2SiO
3Or mixture both, the compound that contains Ce is cerium oxide CeO
2Or cerous nitrate Ce (NO
3)
3Or mixture both.
6. the preparation method of a kind of cerium ion-doped silicate blue fluorescent powder according to claim 2, it is characterized in that: described reducing atmosphere is provided by the mixed gas of gac or hydrogen and nitrogen.
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|---|---|---|---|
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103571461A (en) * | 2013-11-04 | 2014-02-12 | 衢州奥仕特照明有限公司 | Rare earth silicate blue-yellow fluorescent material for high-color-rendering energy saving lamp and preparation method |
| CN103881703A (en) * | 2014-03-25 | 2014-06-25 | 陕西科技大学 | Preparation method of single-substrate fluorescent powder for white-light LED |
-
2013
- 2013-01-24 CN CN2013100279655A patent/CN103087709A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 徐光青等: "Ce3+掺杂片状Sr2MgSi2O7的合成及发光性能", 《硅酸盐学报》 * |
| 章少华等: "Ce3+掺杂和Y3+掺杂对Ca2MgSi2O7:Eu2+荧光粉发光性能的影响", 《材料导报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103571461A (en) * | 2013-11-04 | 2014-02-12 | 衢州奥仕特照明有限公司 | Rare earth silicate blue-yellow fluorescent material for high-color-rendering energy saving lamp and preparation method |
| CN103881703A (en) * | 2014-03-25 | 2014-06-25 | 陕西科技大学 | Preparation method of single-substrate fluorescent powder for white-light LED |
| CN103881703B (en) * | 2014-03-25 | 2016-04-06 | 陕西科技大学 | A kind of preparation method of white light LEDs single-matrix fluorescent material |
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Application publication date: 20130508 |