CN105838369B - A kind of orange red fluorescent powder and preparation method thereof - Google Patents
A kind of orange red fluorescent powder and preparation method thereof Download PDFInfo
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- CN105838369B CN105838369B CN201610227201.4A CN201610227201A CN105838369B CN 105838369 B CN105838369 B CN 105838369B CN 201610227201 A CN201610227201 A CN 201610227201A CN 105838369 B CN105838369 B CN 105838369B
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
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Abstract
A kind of orange red fluorescent powder and preparation method thereof, belongs to luminescent material technical field.The chemical general formula of the orange red fluorescent powder is：DR1‑xCexScO4；Wherein, 0 ＜ x ＜ 1；The D is at least one of Mg, Ca and Sr etc., and wherein Sr is necessary；The R is at least one of La, Y and Lu etc., and wherein La is necessary.The preparation method of the orange red fluorescent powder is as follows：D presomas, R presomas, Ce presomas are mixed with Sc presomas, it is DR to carry out high temperature solid state reaction to get chemical general formula1‑xCexScO4Orange red fluorescent powder.With completely new chemical composition, with Ce3+For activator, which can emit orange light under blue light excitation, so as to make the fluorescent powder that can blue light be converted into orange light, so as to convert white light LEDs applied to yellow fluorescent powder, and improve its colour rendering.
Description
Technical field
The invention belongs to luminescent material technical field, more particularly, to a kind of orange red fluorescent powder and preparation method thereof.
Background technology
It is converted by LED and realizes that white light is mainly the following mode：
1) multi-chip LED.RGB three-primary color LEDs chip packages is generated into white light together.It is combined using RGB three-color LEDs
The technology for forming white light LEDs is most efficient, avoids energy caused by Stokes shift in light-emitting phosphor transfer process
Loss, can obtain highest luminous efficiency, while the light intensity of 3 kinds of different photochromic LED can be separately controlled, realize Full-color color-changing
Effect.But white light LEDs made of this method is each photochromic inconsistent with driving current and temperature change, attenuation speed at any time
Degree also differs, and its heat dissipation problem, also than more prominent, production cost remains high.
2) three primary colors fluorescent powder conversion LED.Three primary colors fluorescent powder conversion LED can under the premise of higher photoluminescence efficiency,
The colour rendering of LED is effectively promoted, it has higher luminous efficacy and colour rendering index.Three primary colours white light LEDs are realized common
Method is to excite one group of yellow, green, blue (RGB) three primary colours fluorescence that can be effectively excited by ultraviolet light using ultraviolet light (UV) LED
Powder, feature are generated for the visible light part of spectrum by fluorescence point completely.But, it has the following disadvantages：Electric light transformation efficiency
It is relatively low；Powder mixing is more difficult, there is efficient fluorescent powder yet-to-be developed；Encapsulating material easy aging, longevity under ultraviolet light
Life is shorter, and there are the hidden danger of ultraviolet light leakage；Highly efficient power type UVLED is not easy to prepare.
3) yellow fluorescent powder conversion LED.Blue light GaN chips+doping Ce at present3+, Yellow light-emitting low temperature yttrium-aluminium-garnet
(Y3Al5O12:Ce3+, YAG) and fluorescent powder is most common two primary colours fluorescent powder conversion LED.As currently commercially most ripe, most
White light LED technology easy to implement has many advantages, such as that energy consumption is small, small, light-weight, compact-sized and causes people's
Extensive concern.In the apparatus, the blue light that GaN is sent out excites YAG and obtains sodium yellow, unabsorbed blue light and yellow light
It is compound to obtain white light, therefore be that the maximum one kind of current usage amount is glimmering in the YAG fluorescent powder of blue light or purple light excited lower Yellow light-emitting low temperature
Light powder.But due to lacking feux rouges in the spectrum of yellow fluorescent powder conversion LED, so the colour rendering of such LED is poor, object exists
Such lower presented color of light source irradiation has certain with the color that object is presented under natural light (sunlight) irradiation
Deviation.
Certainly (orange) red fluorescence powder is suitably added in yellow fluorescent powder, yellow fluorescent powder conversion can be significantly improved
The colour rendering of white light LEDs.
SrLnScO4(Ln=La, Ce, Pr, Nd and Sm) is the material that space group corresponding to a paracrystalline organizations is Abma
(Rina Patel, Charles Simon and Mark T.Weller, Journal of Solid State Chemistry,
Vol.180, No.1,349-359,2007), commonly used in doing dielectric ceramic, purposes belongs to not this material with the present patent application
Same technical field.
Japan Patent JPH04132653 discloses a kind of humidity sensor material, and ingredient includes SrLaScO4, but its purposes with
The present patent application belongs to different technical fields.
At present, SrLnScO4(Ln=La, Ce, Pr, Nd and Sm) commonly used in doing dielectric ceramic or sensor material, also not
See it about the application in terms of luminescent material.
Invention content
An object of the present invention is to provide a kind of orange red fluorescent powder.
It is a further object of the present invention to provide a kind of preparation methods of orange red fluorescent powder.
Shown in the chemical general formula of the orange red fluorescent powder such as formula (I)：
DR1-xCexScO4(I)；
Wherein, 0 ＜ x ＜ 1；The D is at least one of Mg, Ca and Sr etc., and wherein Sr is necessary；The R for La,
Y, at least one of Lu etc., wherein La are necessary.
Preferably, the x is 0.02~0.5.
The preparation method of the orange red fluorescent powder is as follows：
D presomas, R presomas, Ce presomas with Sc presomas are mixed, it is logical to get chemistry to carry out high temperature solid state reaction
Fluorescent powder of the formula as shown in formula (I)；
DR1-xCexScO4(I)；
The molar ratio of D, R, Ce, Sc are 1: (1-x): x in the D presomas, R presomas, Ce presomas, Sc presomas:
1；0 ＜ x ＜ 1；The D is at least one of Mg, Ca, Sr etc., and wherein Sr is necessary；The R in La, Y, Lu etc. extremely
Few one kind, wherein La is necessary.
Preferably, the D presomas, R presomas, Ce presomas and the purity of Sc presomas are not less than 99.5%.
Preferably, the D presomas be the carbonate of D, in nitrate etc. of the oxide of D, the oxalates of D, D at least
It is a kind of；
The R presomas are at least one of nitrate of the carbonate of R, the oxide of R, the oxalates of R, R etc.；
The Ce presomas are at least one in nitrate of the carbonate of Ce, the oxide of Ce, the oxalates of Ce, Ce etc.
Kind；
The Sc presomas are at least one in nitrate of the carbonate of Sc, the oxide of Sc, the oxalates of Sc, Sc etc.
Kind.
The high temperature solid state reaction can be used after compression, carry out high temperature sintering in a reducing atmosphere.
The reducing atmosphere can be ammonia or nitrogen hydrogen mixeding gas；The temperature of the high temperature sintering can be 1250~1550
℃；The time of the high temperature sintering can be 4~10h.
The present invention provides a kind of orange red fluorescent powders and preparation method thereof.The chemical composition of the fluorescent powder is DR1- xCexScO4；Wherein, 0 ＜ x ＜ 1；D is at least one of Mg, Ca and Sr etc., and wherein Sr is necessary；R is La, Y and Lu etc.
At least one of, wherein La is necessary.It is an advantage of the invention that fluorescent powder of the present invention has completely new chemical composition, with
Ce3+For activator, which can emit orange light under blue light excitation, orange red so as to make the fluorescent powder that can be converted into blue light
Light so as to convert white light LEDs applied to yellow fluorescent powder, and improves its colour rendering.
Description of the drawings
Fig. 1 is the X ray diffracting spectrum of fluorescent powder obtained in the embodiment of the present invention 1；
Fig. 2 is the exciting light spectrogram of fluorescent powder obtained in the embodiment of the present invention 1；
Fig. 3 is the launching light spectrogram of fluorescent powder obtained in the embodiment of the present invention 1；
Fig. 4 is the exciting light spectrogram of fluorescent powder obtained in the embodiment of the present invention 2；
Fig. 5 is the launching light spectrogram of fluorescent powder obtained in the embodiment of the present invention 2；
Fig. 6 is the exciting light spectrogram of fluorescent powder obtained in the embodiment of the present invention 3；
Fig. 7 is the launching light spectrogram of fluorescent powder obtained in the embodiment of the present invention 3；
Fig. 8 is the exciting light spectrogram of fluorescent powder obtained in the embodiment of the present invention 4；
Fig. 9 is the launching light spectrogram of fluorescent powder obtained in the embodiment of the present invention 4；
Figure 10 is the exciting light spectrogram of fluorescent powder obtained in the embodiment of the present invention 5；
Figure 11 is the launching light spectrogram of fluorescent powder obtained in the embodiment of the present invention 5.
Specific embodiment
Below in conjunction with embodiment and attached drawing, technical scheme of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art can also make other embodiment.
The present invention provides a kind of orange red fluorescent powder, the chemical general formula such as formula (I) of the fluorescent powder is shown：
DR1-xCexScO4(I)；
Wherein, 0 ＜ x ＜ 1, preferably 0.02~0.5, more preferably 0.02~0.05, in some realities provided by the invention
It applies in example, the x is preferably 0.02；In some embodiments provided by the invention, the x is preferably 0.05；It is carried in the present invention
In some embodiments supplied, the x is preferably 0.1；In other embodiments provided by the invention, the x is preferably 0.5；
The D is at least one of Mg, Ca and Sr etc., and wherein Sr is necessary；In some embodiments provided by the invention, it is described
D is preferably Sr；In some embodiments provided by the invention, the D is preferably Sr and Mg；In some implementations provided by the invention
In example, the D is preferably Sr and Ca；In other embodiments provided by the invention, the D is preferably Sr and Mg and Ca.Institute
R is stated as at least one of La, Y and Lu etc., wherein La is necessary；In some embodiments provided by the invention, the R is excellent
It is selected as La；In some embodiments provided by the invention, the R is preferably La and Y；In other embodiments provided by the invention
In, the R is preferably La and Y and Lu.
Fluorescent powder of the present invention is with Ce3+For activator, which launches orange light under blue light excitation, so as to make this glimmering
Blue light can be converted orange light by light powder, so as to convert white light LEDs applied to yellow fluorescent powder, and improve its colour rendering.
The present invention also provides a kind of preparation method of above-mentioned fluorescent powder, including：By D presomas, R presomas, Ce forerunner
Body is mixed with Sc presomas, is carried out high temperature solid state reaction, is obtained fluorescent powder；
The molar ratio of D, R, Ce and Sc are 1 in the D presomas, R presomas, Ce presomas and Sc presomas：(1-x)：
x：1；0 ＜ x ＜ 1；The D is at least one of Mg, Ca and Sr etc., and wherein Sr is necessary；The R is in La, Y and Lu etc.
At least one, wherein La is necessary.
Wherein, the x and D and R are same as above, and details are not described herein.
The compound for including D that the D presomas are well known in the art has no special limitation, excellent in of the invention
It is selected as at least one of nitrate of the carbonate of D, the oxide of D, the oxalates of D and D etc., the more preferably carbonate of D；
The R presomas are the carbonate of R, the oxide of R, the oxalates of R and R at least one of nitrate etc., more preferably R
Oxide；The Ce presomas are the carbonate of Ce, the oxide of Ce, the oxalates of Ce and Ce nitrate etc. at least
The oxide of one kind, more preferably Ce；The Sc presomas are the carbonate of Sc, the oxide of Sc, the oxalates of Sc and Sc's
The oxide of at least one of nitrate etc., more preferably Sc.
The D presomas, R presomas, Ce presomas and the purity of Sc presomas are preferably not less than each independently
99.5%, purity is higher, and the impurity of obtained fluorescent powder is fewer.
D presomas, R presomas, Ce presomas are mixed with Sc presomas, it is preferred to use grinding is mixed；After mixing,
It is preferred that carrying out tabletting, more preferably tabletting is carried out after drying；The pressure of the tabletting is preferably 1~3MPa.
After tabletting, high temperature sintering is carried out in a reducing atmosphere；The reducing atmosphere is well known to those skilled in the art dry
Pathogenic dryness atmosphere has no special limitation, is preferably ammonia or nitrogen hydrogen mixeding gas in the present invention；The temperature of the high temperature sintering
Preferably 1250~1550 DEG C, more preferably 1300~1450 DEG C are further preferably 1300~1400 DEG C；Provided by the invention one
In a little embodiments, the temperature of the high temperature sintering is preferably 1300 DEG C；In some embodiments provided by the invention, the high temperature
The temperature of sintering is preferably 1400 DEG C；In other embodiments provided by the invention, the temperature of the high temperature sintering is preferably
1450℃。
The time of the high temperature sintering is preferably 4~10h, more preferably 5~8h；In some embodiments provided by the invention
In, the time of the high temperature sintering is preferably 5h；In other embodiments provided by the invention, the time of the high temperature sintering
Preferably 8h.
The high temperature sintering carries out preferably in high temperature furnace；After high temperature sintering, room temperature is cooled to the furnace, you can obtain fluorescence
Powder.
The present invention is with Ce3+For activator, using high temperature solid state reaction, a kind of orange red fluorescent powder is successfully prepared.
In order to further illustrate the present invention, with reference to embodiments to a kind of orange red fluorescent powder provided by the invention and its
Preparation method is described in detail.
Reagent used in following embodiment is commercially available.
Embodiment 1
Raw material is SrCO3(analysis is pure), La2O3(analysis is pure), CeO2(99.99%) and Sc2O3(analysis is pure), molar ratio is
1: 0.49: 0.02: 0.5, above-mentioned raw materials are ground, dry after 2MPa pressure lower sheeting, be packed into crucible, ammonia reduction
Under atmosphere, in high temperature furnace, 1450 DEG C of sintering 5h, furnace cooling to room temperature, obtaining theoretical chemistry ingredient is
SrLa0.98Ce0.02ScO4Fluorescent powder.
The fluorescent material obtained in embodiment 1 is analyzed using X-ray diffraction, obtains its X ray diffracting spectrum, such as
Shown in Fig. 1.
The fluorescent material obtained in embodiment 1 is analyzed using Fluorescence Spectrometer, obtains its exciting light spectrogram, is such as schemed
Shown in 2.It can be seen that the excitation band of the fluorescent material is mainly fallen in blue light region.
The fluorescent material obtained in embodiment 1 is analyzed using Fluorescence Spectrometer, obtains its launching light spectrogram, is such as schemed
Shown in 3.It can be seen that the material can effectively be stimulated by blue light and emit orange light, so as to which blue light can be converted into orange by the fluorescent material
Feux rouges.
Embodiment 2
Raw material is SrCO3(analysis is pure), La2O3(analysis is pure), CeO2(99.99%) and Sc2O3(analysis is pure), molar ratio is
1: 0.25: 0.5: 0.5, above-mentioned raw materials are ground, dry after 1MPa pressure lower sheeting, be packed into crucible, ammonia reduction
Under atmosphere, in high temperature furnace, 1450 DEG C of sintering 5h, furnace cooling to room temperature, obtaining theoretical chemistry ingredient is
SrLa0.5Ce0.5ScO4Fluorescent powder.
The fluorescent material obtained in embodiment 2 is analyzed using Fluorescence Spectrometer, obtains its exciting light spectrogram, is such as schemed
Shown in 4.It can be seen that the excitation band of the fluorescent powder is mainly fallen in blue light region.
The fluorescent material obtained in embodiment 2 is analyzed using Fluorescence Spectrometer, obtains its launching light spectrogram, is such as schemed
Shown in 5.It can be seen that the fluorescent powder can effectively be stimulated by blue light and emit orange light, so as to which blue light can be converted into orange by the fluorescent powder
Feux rouges.
Embodiment 3
Raw material is SrCO3(analysis is pure), MgCO3(analysis is pure), La2O3(analysis is pure), Y2O3(analysis is pure), CeO2
(99.99%) and Sc2O3(analysis is pure), molar ratio 0.95: 0.05: 0.45: 0.025: 0.05: 0.5 grinds above-mentioned raw materials
Mixing, it is dry after 3MPa pressure lower sheeting, be packed into crucible, under the reducing atmosphere of nitrogen and hydrogen mixture, in high temperature furnace, 1450
DEG C sintering 5h, furnace cooling to room temperature, obtain theoretical chemistry ingredient be Sr0.95Mg0.05La0.9Y0.05Ce0.05ScO4Fluorescent powder.
The fluorescent material obtained in embodiment 3 is analyzed using Fluorescence Spectrometer, obtains its exciting light spectrogram, is such as schemed
Shown in 6.It can be seen that the excitation band of the fluorescent powder is mainly fallen in blue light region.
The fluorescent material obtained in embodiment 3 is analyzed using Fluorescence Spectrometer, obtains its launching light spectrogram, is such as schemed
Shown in 7.It can be seen that the fluorescent powder can effectively be stimulated by blue light and emit orange light, so as to which blue light can be converted into orange by the fluorescent powder
Feux rouges.
Embodiment 4
Raw material is SrCO3(analysis is pure), CaCO3(analysis is pure), La2O3(analysis is pure), Y2O3(analysis is pure), CeO2
(99.99%) and Sc2O3(analysis is pure), molar ratio 0.9: 0.1: 0.35: 0.1: 0.1: 0.5, above-mentioned raw materials are ground,
In the pressure lower sheeting of 1.5MPa after drying, it is packed into crucible, under ammonia reducing atmosphere, in high temperature furnace, 1400 DEG C of sintering 8h, with
Stove is cooled to room temperature, obtains theoretical chemistry ingredient as Sr0.9Ca0.1La0.7Y0.2Ce0.1ScO4Fluorescent powder.
The fluorescent material obtained in embodiment 4 is analyzed using Fluorescence Spectrometer, obtains its exciting light spectrogram, is such as schemed
Shown in 8.It can be seen that the excitation band of the fluorescent powder is mainly fallen in blue light region.
The fluorescent material obtained in embodiment 4 is analyzed using Fluorescence Spectrometer, obtains its launching light spectrogram, is such as schemed
Shown in 9.It can be seen that the fluorescent powder can effectively be stimulated by blue light and emit orange light, so as to which blue light can be converted into orange by the fluorescent powder
Feux rouges.
Embodiment 5
Raw material is SrCO3(analysis is pure), MgCO3(analysis is pure), CaCO3(analysis is pure), La2O3(analysis is pure), Y2O3(analysis
It is pure), Lu2O3(analysis is pure), CeO2(99.99%) and Sc2O3(analysis is pure), molar ratio 0.9: 0.05: 0.05: 0.4: 0.04:
0.05: 0.02: 0.5, raw material is ground, dry after 2.5MPa pressure lower sheeting, be packed into crucible, ammonia reducing atmosphere
Under, in high temperature furnace, 1300 DEG C of sintering 5h, furnace cooling to room temperature, obtaining theoretical chemistry ingredient is
Sr0.9Mg0.05Ca0.05La0.8Y0.08Lu0.1Ce0.02ScO4Fluorescent powder.
The fluorescent material obtained in embodiment 5 is analyzed using Fluorescence Spectrometer, obtains its exciting light spectrogram, is such as schemed
Shown in 10.It can be seen that the excitation band of the fluorescent powder is mainly fallen in blue light region.
The fluorescent material obtained in embodiment 5 is analyzed using Fluorescence Spectrometer, obtains its launching light spectrogram, is such as schemed
Shown in 11.It can be seen that the fluorescent powder can effectively be stimulated by blue light and emit orange light, so as to which blue light can be converted by the fluorescent powder
Orange light.
Claims (10)
1. a kind of orange red fluorescent powder, it is characterised in that shown in its chemical general formula such as formula (I)：
DR1-xCexScO4(I)；
Wherein, 0 ＜ x ＜ 1；The D is at least one of Mg, Ca and Sr, and wherein Sr is necessary；The R is in La, Y, Lu
At least one, wherein La is necessary.
2. a kind of orange red fluorescent powder as described in claim 1, it is characterised in that the x is 0.02~0.5.
3. a kind of preparation method of orange red fluorescent powder as described in claim 1, it is characterised in that it is as follows：
D presomas, R presomas, Ce presomas are mixed with Sc presomas, carry out high temperature solid state reaction to get chemical general formula such as
Fluorescent powder shown in formula (I)；
DR1-xCexScO4 (I)。
4. a kind of preparation method of orange red fluorescent powder as claimed in claim 3, it is characterised in that the D presomas, R forerunner
The molar ratio of D, R, Ce, Sc are 1 in body, Ce presomas, Sc presomas: (1-x): x: 1；0 ＜ x ＜ 1；The D is Mg, Ca, Sr
At least one of, wherein Sr is necessary；The R is at least one of La, Y, Lu, and wherein La is necessary；Before the D
The purity of body, R presomas, Ce presomas, Sc presomas is driven not less than 99.5%.
5. a kind of preparation method of orange red fluorescent powder as claimed in claim 3, it is characterised in that the D presomas are the carbon of D
Hydrochlorate, the oxide of D, the oxalates of D, D at least one of nitrate.
6. a kind of preparation method of orange red fluorescent powder as claimed in claim 3, it is characterised in that the R presomas are the carbon of R
Hydrochlorate, the oxide of R, the oxalates of R, R at least one of nitrate.
7. a kind of preparation method of orange red fluorescent powder as claimed in claim 3, it is characterised in that the Ce presomas are Ce's
Carbonate, the oxide of Ce, the oxalates of Ce, Ce at least one of nitrate.
8. a kind of preparation method of orange red fluorescent powder as claimed in claim 3, it is characterised in that the Sc presomas are Sc's
Carbonate, the oxide of Sc, the oxalates of Sc, Sc at least one of nitrate.
9. a kind of preparation method of orange red fluorescent powder as claimed in claim 3, it is characterised in that the high temperature solid state reaction is adopted
With after compression, high temperature sintering is carried out in a reducing atmosphere.
10. a kind of preparation method of orange red fluorescent powder as claimed in claim 9, it is characterised in that the reducing atmosphere is ammonia
Or nitrogen hydrogen mixeding gas；The temperature of the high temperature sintering can be 1250~1550 DEG C；The time of the high temperature sintering can be 4~
10h。
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1981018A (en) * | 2004-06-30 | 2007-06-13 | 三菱化学株式会社 | Fluorescent substance, light-emitting element using the same, image display device, and illuminating device |
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| JPH04132653A (en) * | 1990-09-25 | 1992-05-06 | Mitsubishi Kasei Corp | Humidity sensor element |
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| CN1981018A (en) * | 2004-06-30 | 2007-06-13 | 三菱化学株式会社 | Fluorescent substance, light-emitting element using the same, image display device, and illuminating device |
Non-Patent Citations (1)
| Title |
|---|
| LnSrScO4 ( Ln= La, Ce, Pr, Nd and Sm) systems and structurecorrelations for A2BO4 (K2NiF4) structure types;Rina Patel等;《Journal of Solid State Chemistry》;20071231;第180卷;349-359 * |
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