CN104119870A - Praseodymium and ytterbium co-doped alumina up-conversion luminescent material and preparation method and application thereof - Google Patents
Praseodymium and ytterbium co-doped alumina up-conversion luminescent material and preparation method and application thereof Download PDFInfo
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- CN104119870A CN104119870A CN201310150187.9A CN201310150187A CN104119870A CN 104119870 A CN104119870 A CN 104119870A CN 201310150187 A CN201310150187 A CN 201310150187A CN 104119870 A CN104119870 A CN 104119870A
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- luminescent material
- conversion luminescent
- aluminum oxide
- praseodymium
- ytterbium codoped
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Abstract
A praseodymium and ytterbium co-doped alumina up-conversion luminescent material has the following chemical general formula of Al2O3:xPr<3+>, yYb <3+>, wherein x is 0.01-0.08 and y is 0.01-0.06. In a photoluminescence spectrum of the praseodymium and ytterbium co-doped alumina up-conversion luminescent material, the excitation wavelength of the praseodymium and ytterbium co-doped alumina up-conversion luminescent material is 578 nm, in a wavelength region of 483 nm, luminescence peaks can be produced by transition radiation from <3>P0 to <3>H4 of Pr<3+> ions, and the praseodymium and ytterbium co-doped alumina up-conversion luminescent material can be used as a blue light luminescent material. The invention also provides a preparation method of the praseodymium and ytterbium co-doped alumina up-conversion luminescent material, and organic light-emitting diodes using the praseodymium and ytterbium co-doped alumina up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material, preparation method and Organic Light Emitting Diode.
Background technology
Organic Light Emitting Diode (OLED) because unit construction is simple, the characteristic such as cheap, the luminous of production cost, reaction times be short, flexible, and obtained the utmost point, apply widely.But owing to obtaining at present, the OLED blue light material of stability and high efficiency is more difficult, has limited greatly the development of white light OLED device and light source industry.
Upconverting fluorescent material can be launched visible ray under long wave (as infrared) radiation excitation, even UV-light, is with a wide range of applications in fields such as optical fiber communication technology, fibre amplifier, 3 D stereo demonstration, biomolecules fluorescence labelling, infrared detectives.But, can be by infrared, the long-wave radiations such as red-green glow inspire the praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material of blue emission, have not yet to see report.
Summary of the invention
Based on this, being necessary to provide a kind of can be inspired praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material, the preparation method of blue light and be used the Organic Light Emitting Diode of this praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material by long-wave radiation.
A praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material, its chemical formula is Al
2o
3: xPr
3+, yYb
3+, wherein, x is that 0.01～0.08, y is 0.01～0.06.
Described x is that 0.05, y is 0.03.
A preparation method for praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material, comprises the following steps
Step 1, according to Al
2o
3: xPr
3+, yYb
3+the stoichiometric ratio of each element takes Al
2o
3, Pr
2o
3and Yb
2o
3powder, wherein, x is that 0.01～0.08, y is 0.01～0.06;
Step 2, the powder taking in described step 1 is mixed and obtains presoma;
Step 3, by the calcination 0.5 hour～5 hours at 800 ℃～1000 ℃ of the presoma in described step 2,
Step 4, the precursor after processing in described step 3 is cooled to 100 ℃～500 ℃, then is incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is Al
2o
3: xPr
3+, yYb
3+praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material.
Described Al
2o
3, Pr
2o
3and Yb
2o
3each component mol ratio of powder is (0.86～0.98): (0.01～0.08): (0.01～0.06).
Described Al
2o
3, Pr
2o
3and Yb
2o
3each component mol ratio of powder is 0.92:0.05:0.03.
Described in step 2, mixing is described powder to be ground in corundum alms bowl 20 minutes～60 minutes.
In step 3 by the calcination 3 hours at 950 ℃ of described presoma.
Cooling temperature in step 4 is 250 ℃, and soaking time is 2 hours.
A kind of Organic Light Emitting Diode, comprise the substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer that stack gradually, it is characterized in that, in described transparent encapsulated layer, be dispersed with praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material, the chemical formula of described praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material is Al
2o
3: xPr
3+, yYb
3+, wherein, x is that 0.01～0.08, y is 0.01～0.06.
X is that 0.05, y is 0.03.
The preparation method of above-mentioned praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material is comparatively simple, and cost is lower, produces comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material of preparation, the excitation wavelength of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation form glow peak, can be used as blue light emitting material.
Accompanying drawing explanation
Fig. 1 is the structural representation of the Organic Light Emitting Diode of an embodiment.
Fig. 2 is the photoluminescence spectrogram of the praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material of embodiment 1 preparation.
Fig. 3 is the XRD spectrum of the praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material of embodiment 1 preparation.
Fig. 4 forms the spectrogram of the Organic Light Emitting Diode emitting white light doped with praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material in the transparent encapsulated layer of embodiment 1 preparation.
Embodiment
Below in conjunction with the drawings and specific embodiments, praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material and preparation method thereof is further illustrated.
The praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material of one embodiment, its chemical formula is Al
2o
3: xPr
3+, yYb
3+, wherein, x is that 0.01～0.08, y is 0.01～0.06.
Preferably, x is that 0.05, y is 0.03.
In the photoluminescence spectra of this praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material, the excitation wavelength of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material is 578nm, when material is subject to long wavelength's (as 578nm) radiation, and Pr
3+ion just in
3p
0excited state, then to
3h
4transition, just sends the blue light of 483nm, can be used as blue light emitting material.
The preparation method of above-mentioned praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material, comprises the following steps:
Step S11, according to Al
2o
3: xPr
3+, yYb
3+the stoichiometric ratio of each element takes Al
2o
3, Pr
2o
3and Yb
2o
3powder, wherein, x is that 0.01～0.08, y is 0.01～0.06.
In this step, described Al
2o
3, Pr
2o
3and Yb
2o
3each component mol ratio of powder is (0.86～0.98): (0.01～0.08): (0.01～0.06).
In this step, preferred, described Al
2o
3, Pr
2o
3and Yb
2o
3each component mol ratio of powder is 0.92:0.05:0.03.
Step S13, the powder taking in step S11 is mixed and obtains presoma.
In this step, powder is ground in corundum alms bowl to the 20 minutes～presoma that obtains mixing for 60 minutes, preferably grind 40 minutes.
Step S15, by presoma calcination 0.5 hour～5 hours at 800 ℃～1000 ℃,
Preferably, presoma calcination 3 hours at 950 ℃.
After step S17, the precursor after will be in step S15 processing, be cooled to 100 ℃～500 ℃, then be incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is Al
2o
3: xPr
3+, yYb
3+, wherein, x is that 0.01～0.08, y is 0.01～0.06.
Preferably, the precursor after processing in step S15 is cooled to 500 ℃, then is incubated 2 hours.
The preparation method of above-mentioned praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material is comparatively simple, and cost is lower, produces comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material of preparation, the excitation wavelength of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation form glow peak, can be used as blue light emitting material.
Refer to Fig. 1, the Organic Light Emitting Diode 100 of an embodiment, this Organic Light Emitting Diode 100 comprises substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the transparent encapsulated layer 5 stacking gradually.In transparent encapsulated layer 5, be dispersed with praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material 6, the chemical formula of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material is Al
2o
3: xPr
3+, yYb
3+, wherein, x is 0.01～0.08, y is 0.01～0.06, organic luminous layer 3 in this device sends red-green glow, and part red-green glow excites and in transparent encapsulated layer 5, is dispersed with praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material 6 and sends blue light, and last redgreenblue just blendes together white light.
Be specific embodiment below.
Embodiment 1
Selecting purity is 99.99% powder, by Al
2o
3, Pr
2o
3and Yb
2o
3each component of powder is 0.92mmol by mole number, 0.05mmol, 0.03mmol grinds and it was evenly mixed in 40 minutes in corundum mortar, then calcination 3 hours at 950 ℃ in retort furnace, then be cooled to 250 ℃ of insulations 2 hours, furnace cooling takes out to room temperature again, obtains block materials, and after pulverizing, can obtain chemical general formula is Al
2o
3: 0.05Pr
3+, 0.03Yb
3+up-conversion phosphor.
Process prepared by Organic Light Emitting Diode
The substrate 1 stacking gradually uses soda-lime glass, negative electrode 2 to use metal A g layer, organic luminous layer 3 to use Ir (piq) 2 (acac) Chinese name to close iridium (III), transparent anode 4 use tin indium oxide ITO two (1-phenyl-isoquinoline 99.9) (methyl ethyl diketones), and transparent encapsulated layer 5 tetrafluoroethylene.In transparent encapsulated layer 5, be dispersed with praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material 6, the chemical formula of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material is Al
2o
3: 0.05Pr
3+, 0.03Yb
3+.
Refer to Fig. 2, Figure 2 shows that the photoluminescence spectra figure of the praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material obtaining.As seen from Figure 2, the excitation wavelength of the praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material that the present embodiment obtains is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation form glow peak, this praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material can be used as blue light emitting material.
Refer to Fig. 3, in Fig. 3, curve is for implementing the XRD curve of the praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material of 1 preparation, test comparison standard P DF card.Contrast PDF card, can see that the diffraction peak in publishing picture is the peak crystallization of aluminum oxide, does not occur the diffraction peak of doped element and other impurity; Illustrate that the product that this preparation method obtains has good crystalline quality.
Refer to Fig. 4, Fig. 4 curve 1 is for form the spectrogram of the Organic Light Emitting Diode emitting white light in transparent encapsulated layer doped with praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material, and curve 2 is not doped with the contrast of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material in transparent encapsulated layer.In figure, can find out, fluorescent material can inspire the blue light of shortwave by the red light of long wave, blendes together white light.
Embodiment 2
Selecting purity is 99.99% powder, by Al
2o
3, Pr
2o
3and Yb
2o
3each component of powder is 0.98mmol by mole number, 0.01mmol, 0.01mmol grinds and it was evenly mixed in 20 minutes in corundum mortar, then calcination 3 hours at 800 ℃ in retort furnace, then be cooled to 100 ℃ of insulations 3 hours, furnace cooling takes out to room temperature again, obtains block materials, and after pulverizing, can obtain chemical general formula is Al
2o
3: 0.01Pr
3+, 0.01Yb
3+up-conversion phosphor.
Embodiment 3
Selecting purity is 99.99% powder, by Al
2o
3, Pr
2o
3and Yb
2o
3each component of powder is 0.86mmol by mole number, 0.08mmol, 0.06mmol, in corundum mortar, grind and it was evenly mixed in 60 minutes, then calcination 3 hours at 1000 ℃ in retort furnace, be then cooled to 500 ℃ of insulations 0.5 hour, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is Al
2o
3: 0.08Pr
3+, 0.06Yb
3+up-conversion phosphor.
Embodiment 4
Selecting purity is 99.99% powder, by Al
2o
3, Pr
2o
3and Yb
2o
3each component of powder is 0.93mmol by mole number, 0.02mmol, 0.05mmol grinds and it was evenly mixed in 30 minutes in corundum mortar, then calcination 3 hours at 900 ℃ in retort furnace, then be cooled to 250 ℃ of insulations 2 hours, furnace cooling takes out to room temperature again, obtains block materials, and after pulverizing, can obtain chemical general formula is Al
2o
3: 0.02Pr
3+, 0.05Yb
3+up-conversion phosphor.
Embodiment 5
Selecting purity is 99.99% powder, by Al
2o
3, Pr
2o
3and Yb
2o
3each component of powder is 0.92mmol by mole number, 0.06mmol, 0.02mmol, in corundum mortar, grind and it was evenly mixed in 60 minutes, then calcination 2 hours at 800 ℃ in retort furnace, be then cooled to 100 ℃ of insulations 3 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is Al
2o
3: 0.06Pr
3+, 0.02Yb
3+up-conversion phosphor.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material, is characterized in that: its chemical general formula is Al
2o
3: xPr
3+, yYb
3+, wherein, x is that 0.01～0.08, y is 0.01～0.06.
2. praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material according to claim 1, is characterized in that, described x is that 0.05, y is 0.03.
3. a preparation method for praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material, is characterized in that, comprises the following steps:
Step 1, according to Al
2o
3: xPr
3+, yYb
3+the stoichiometric ratio of each element takes Al
2o
3, Pr
2o
3and Yb
2o
3powder, wherein, x is that 0.01～0.08, y is 0.01～0.06;
Step 2, the powder taking in described step 1 is mixed and obtains presoma;
Step 3, by the calcination 0.5 hour～5 hours at 800 ℃～1000 ℃ of described presoma,
Step 4, the precursor after processing in described step 3 is cooled to 100 ℃～500 ℃, then is incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is Al
2o
3: xPr
3+, yYb
3+praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material.
4. the preparation method of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material according to claim 3, is characterized in that described Al
2o
3, Pr
2o
3and Yb
2o
3each component mol ratio of powder is (0.86～0.98): (0.01～0.08): (0.01～0.06).
5. the preparation method of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material according to claim 3, is characterized in that described Al
2o
3, Pr
2o
3and Yb
2o
3each component mol ratio of powder is 0.92:0.05:0.03.
6. the preparation method of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material according to claim 3, is characterized in that, described in step 2, mixing is described powder to be ground in corundum alms bowl 20 minutes～60 minutes.
7. the preparation method of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material according to claim 3, is characterized in that, in step 3 by the calcination 3 hours at 950 ℃ of described presoma.
8. the preparation method of praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material according to claim 3, is characterized in that, the cooling temperature in step 4 is 250 ℃, and soaking time is 2 hours.
9. an Organic Light Emitting Diode, this Organic Light Emitting Diode comprises substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer stacking gradually, it is characterized in that, in described transparent encapsulated layer, be dispersed with praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material, the chemical formula of described praseodymium ytterbium codoped aluminum oxide up-conversion luminescent material is Al
2o
3: xPr
3+, yYb
3+, wherein, x is that 0.01～0.08, y is 0.01～0.06.
10. Organic Light Emitting Diode according to claim 9, is characterized in that, described x is that 0.05, y is 0.03.
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|---|---|---|---|
| CN201310150187.9A CN104119870A (en) | 2013-04-26 | 2013-04-26 | Praseodymium and ytterbium co-doped alumina up-conversion luminescent material and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310150187.9A CN104119870A (en) | 2013-04-26 | 2013-04-26 | Praseodymium and ytterbium co-doped alumina up-conversion luminescent material and preparation method and application thereof |
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| Publication Number | Publication Date |
|---|---|
| CN104119870A true CN104119870A (en) | 2014-10-29 |
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ID=51765514
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310150187.9A Pending CN104119870A (en) | 2013-04-26 | 2013-04-26 | Praseodymium and ytterbium co-doped alumina up-conversion luminescent material and preparation method and application thereof |
Country Status (1)
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS627958B2 (en) * | 1979-05-25 | 1987-02-19 | Fuji Photo Film Co Ltd | |
| JP3600048B2 (en) * | 1998-11-20 | 2004-12-08 | 株式会社東京化学研究所 | Method for producing aluminate-based phosphor |
-
2013
- 2013-04-26 CN CN201310150187.9A patent/CN104119870A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS627958B2 (en) * | 1979-05-25 | 1987-02-19 | Fuji Photo Film Co Ltd | |
| JP3600048B2 (en) * | 1998-11-20 | 2004-12-08 | 株式会社東京化学研究所 | Method for producing aluminate-based phosphor |
Non-Patent Citations (1)
| Title |
|---|
| 殷海涛: "稀土（Pr3+，Sm3+，Er3+，Yb3+）共掺氧化铝的光学特性", 《中国优秀硕士学位论文全文数据库基础科学辑》 * |
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Application publication date: 20141029 |