CN103059855A - Yttrium oxide phosphors for up-conversion luminescence, and preparation method and application thereof - Google Patents
Yttrium oxide phosphors for up-conversion luminescence, and preparation method and application thereof Download PDFInfo
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- CN103059855A CN103059855A CN2011103203254A CN201110320325A CN103059855A CN 103059855 A CN103059855 A CN 103059855A CN 2011103203254 A CN2011103203254 A CN 2011103203254A CN 201110320325 A CN201110320325 A CN 201110320325A CN 103059855 A CN103059855 A CN 103059855A
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- fluorescent material
- yttrium oxide
- conversion luminescence
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Abstract
The invention belongs to the phosphor field, and discloses yttrium oxide phosphors for up-conversion luminescence, and a preparation method and an application thereof. The phosphors have a structural formula of Y2-x-yO3:xHo3+, yYb3+, wherein Ho3+ and Yb3+ are doping ions; x value ranges from 0.02 to 0.1; and y value ranges from 0.02 to 0.2. The yttrium oxide phosphors for up-conversion luminescence prepared by the invention can excite short-wavelength luminescence of blue light by long-wavelength radiation from infrared to green light, so that the phosphors can make up the insufficiency of blue light materials in present display and luminescent materials.
Description
Technical field
The present invention relates to a kind of fluorescent material, relate in particular to fluorescent material of a kind of yttrium oxide up-conversion luminescence and its preparation method and application.
Background technology
The full name Organic Light Emitting Diode of OLED, Organic Light Emitting Diode.It has a lot of advantages, and its unit construction is simple, and production cost is cheap, and self luminous characteristic adds that the reaction times of OLED is short, and flexible characteristic is more arranged, and makes its range of application extremely wide.But because it is relatively more difficult to obtain at present the OLED blue light material of stability and high efficiency, limited greatly the development of white light OLED device and light source industry.
Upconverting fluorescent material can be launched visible light under long wave (as infrared) radiation excitation, even UV-light, be 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 be prepared into the field that fluorescent material is applied to OLED, still rarely seen report.
Summary of the invention
One of purpose of the present invention is to provide a kind of fluorescent material that can be inspired by long wavelength radiations such as infrared, red-green glows the yttrium oxide up-conversion luminescence of blue emission.
A kind of fluorescent material of yttrium oxide up-conversion luminescence, its structural formula are Y
2-x-yO
3: xHo
3+, yYb
3+Wherein, Ho
3+And Yb
3+Be dopant ion, the span of x is that the span of 0.02～0.1, y is 0.02～0.2; Preferably, x value 0.06, y value 0.1.
Another object of the present invention is to provide the preparation method of the fluorescent material of above-mentioned yttrium oxide up-conversion luminescence, comprise the steps:
Step S1, according to structural formula Y
2-x-yO
3: xHo
3+, yYb
3+In each element chemistry metering ratio, take by weighing powder: Y
2O
3, Ho
2O
3And Yb
2O
3
Step S2, the powder that step S1 is taken by weighing mix, ground 20～60 minutes, obtain the powder presoma;
Step S3, with the powder presoma of step S2 in 800～1000 ℃ of lower calcinings 0.5～5 hour, be cooled to subsequently 100～500 ℃, and after being incubated 0.5～3 hour under this temperature, be cooled to room temperature, obtain block product;
Step S4, the block product among the step S3 is ground, obtain the fluorescent material of described yttrium oxide up-conversion luminescence; The structural formula of this fluorescent material is Y
2-x-yO
3: xHo
3+, yYb
3+Wherein, Ho
3+And Yb
3+Be dopant ion;
Wherein, structural formula Y
2-x-yO
3: xHo
3+, yYb
3+In, the span of x is that the span of 0.02～0.1, y is 0.02～0.2.
Among the preparation method of the fluorescent material of above-mentioned yttrium oxide up-conversion luminescence:
Among the step S2, the milling time of described powder is 40 minutes;
Among the step S3, the calcining temperature of described calcination process is 950 ℃, and calcination time is 3 hours; After calcination process finished, the temperature of described insulating process was 250 ℃, and soaking time is 2 hours;
Structural formula Y
2-x-yO
3: xHo
3+, yYb
3+In, preferred, x value 0.06, y value 0.1.
Another purpose of the present invention is to provide the application of fluorescent material in Organic Light Emitting Diode of above-mentioned yttrium oxide up-conversion luminescence, mainly is the luminescent layer material as Organic Light Emitting Diode.These fluorescent material are to be after the Organic Light Emitting Diode of carrying out monochrome (such as ruddiness) is made, and fluorescent material is mixed in is coated in the Organic Light Emitting Diode outside in the packaged material, are subject to exciting of ruddiness, give off blue light.
The fluorescent material of the yttrium oxide up-conversion luminescence of the present invention's preparation can realize inspiring the blue light shortwave by infrared long-wave radiation to green glow luminous.Therefore, this fluorescent material can remedy the deficiency of blue light material in present demonstration and the luminescent material.
In addition, the preparation method of the fluorescent material of yttrium oxide up-conversion luminescence provided by the invention is simple, with low costly is applicable to production, and reaction process belongs to environmental protection, less energy-consumption, high benefit industry without three industrial wastes.
Description of drawings
Fig. 1 is preparation technology's schema of the fluorescent material of yttrium oxide up-conversion luminescence of the present invention;
Fig. 2 is the electroluminescent spectrum figure of fluorescent material of the yttrium oxide up-conversion luminescence that the Yb element makes of undoping in the fluorescent material of the yttrium oxide up-conversion luminescence that makes of embodiment 1 and the Comparative Examples;
Fig. 3 is the structural representation of the Organic Light Emitting Diode of embodiment 4.
Embodiment
The fluorescent material of a kind of yttrium oxide up-conversion luminescence provided by the invention, its structural formula are Y
2-x-yO
3: xHo
3+, yYb
3+Wherein, Ho
3+And Yb
3+Be dopant ion, the span of x is that the span of 0.02～0.1, y is 0.02～0.2; Preferably, x value 0.06, y value 0.1.
The fluorescent material of the yttrium oxide up-conversion luminescence of the present invention's preparation can realize inspiring the blue light shortwave by infrared long-wave radiation to green glow luminous.Therefore, this fluorescent material can remedy the deficiency of blue light material in present demonstration and the luminescent material.
The preparation method of the fluorescent material of above-mentioned yttrium oxide up-conversion luminescence as shown in Figure 1, comprises the steps:
Step S1, according to structural formula Y
2-x-yO
3: xHo
3+, yYb
3+In each element chemistry metering ratio, take by weighing powder: Y
2O
3, Ho
2O
3And Yb
2O
3
Step S2, the powder that step S1 is taken by weighing mix, ground 20～60 minutes, obtain the powder presoma;
Step S3, with the powder presoma of step S2 in 800～1000 ℃ of lower calcinings 0.5～5 hour, be cooled to subsequently 100～500 ℃, and after being incubated 0.5～3 hour under this temperature, be cooled to room temperature, obtain block product;
Step S4, the block product among the step S3 is ground, obtain the fluorescent material of described yttrium oxide up-conversion luminescence; The structural formula of this fluorescent material is Y
2-x-yO
3: xHo
3+, yYb
3+Wherein, Ho
3+And Yb
3+Be dopant ion;
Wherein, structural formula Y
2-x-yO
3: xHo
3+, yYb
3+In, the span of x is that the span of 0.02～0.1, y is 0.02～0.2.
Among the preparation method of the fluorescent material of above-mentioned yttrium oxide up-conversion luminescence:
Among the step S2, the milling time of described powder is 40 minutes;
Among the step S3, the calcining temperature of described calcination process is 950 ℃, and calcination time is 3 hours; After calcination process finished, the temperature of described insulating process was 250 ℃, and soaking time is 2 hours;
Structural formula Y
2-x-yO
3: xHo
3+, yYb
3+In, preferred, x value 0.06, y value 0.1.
The preparation method of the fluorescent material of yttrium oxide up-conversion luminescence provided by the invention is simple, with low costly is applicable to production, and reaction process belongs to environmental protection, less energy-consumption, high benefit industry without three industrial wastes.
The application of the fluorescent material of above-mentioned yttrium oxide up-conversion luminescence in Organic Light Emitting Diode mainly is the luminescent layer material as Organic Light Emitting Diode.These fluorescent material are to be after the Organic Light Emitting Diode of carrying out monochrome (such as ruddiness) is made, and fluorescent material is mixed in is coated in the Organic Light Emitting Diode outside in the packaged material, are subject to exciting of ruddiness, give off blue light.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
1, selecting purity is 99.99% powder: Y
2O
3, Ho
2O
3And Yb
2O
3Powder, its quality is respectively 2.24g, 0.113g and 0.197g;
2, above-mentioned powder is placed the corundum mortar, grind and made its even mixing in 40 minutes, obtain the powder presoma;
3, the powder presoma is placed retort furnace, 950 ℃ of lower calcinations 3 hours, then is cooled to 250 ℃ of insulations 3 hours, naturally cool to again room temperature and take out block product,
4, block product is ground, pulverizes, obtaining structural formula is Y
1.84O
3: 0.06Ho
3+, 0.1Yb
3+Up-conversion phosphor.
Fig. 2 is the electroluminescent spectrum figure of fluorescent material of the yttrium oxide up-conversion luminescence that the Yb element makes of undoping in the fluorescent material of the yttrium oxide up-conversion luminescence that makes of embodiment 1 and the Comparative Examples; As shown in Figure 2, curve 1 is the photoluminescence spectra of embodiment 1 sample, and excitation wavelength is 640nm; That the glow peak of the 490nm that obtains is corresponding is Ho
3+Ion
5F
3→
5I
8Transition radiation luminous.Curve 2 is to undope under the same preparation condition to mix altogether the Comparative Examples of Yb element.
Embodiment 2
1, selecting purity is 99.99% powder: Y
2O
3, Ho
2O
3And Yb
2O
3Powder, its mass ratio is respectively 2.39g, 0.038g and 0.039g;
2, above-mentioned powder is placed the corundum mortar grind and made its even mixing in 20 minutes, obtain the powder presoma;
3, the powder presoma is placed retort furnace, 800 ℃ of lower calcinations 5 hours, then be cooled to 100 ℃ of insulations 3 hours, naturally cool to again room temperature and take out block product;
4, block product is ground, pulverizes, obtaining structural formula is Y
1.96O
3: 0.02Ho
3+, 0.02Yb
3+Up-conversion phosphor.
Embodiment 3
1, selecting purity is 99.99% powder: Y
2O
3, Ho
2O
3And Yb
2O
3Powder, its quality is respectively 2.07g, 0.150g and 0.394g;
2, above-mentioned powder is placed the corundum mortar grind and made its even mixing in 60 minutes, obtain the powder presoma;
3, the powder presoma is placed retort furnace, 1000 ℃ of lower calcinations 0.5 hour, then be cooled to 500 ℃ of insulations 0.5 hour, naturally cool to again room temperature and take out block product;
4, block product is ground, pulverizes, obtaining structural formula is Y
1.7O
3: 0.1Ho
3+, 0.2Yb
3+Up-conversion phosphor.
Embodiment 4
The present embodiment 4 is Organic Light Emitting Diode, sees also Fig. 3, and the structure of this Organic Light Emitting Diode is substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the transparent encapsulated layer 5 that stacks gradually; Wherein, be dispersed with the fluorescent material 6 that makes among the embodiment 1 in the transparent encapsulated layer 5.
When this Organic Light Emitting Diode used, the part ruddiness excitated fluorescent powder 6 of organic luminous layer 3 sent blue light, this blue light with inspire white light after remaining ruddiness in the luminescent layer 3 mixes.
Should be understood that, above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.
Claims (8)
1. the fluorescent material of a yttrium oxide up-conversion luminescence is characterized in that, the structural formula of this fluorescent material is Y
2-x-yO
3: xHo
3+, yYb
3+Wherein, Ho
3+And Yb
3+Be dopant ion, the span of x is that the span of 0.02～0.1, y is 0.02～0.2.
2. the fluorescent material of yttrium oxide up-conversion luminescence according to claim 1 is characterized in that, x value 0.06, y value 0.1.
3. the preparation method of the fluorescent material of a yttrium oxide up-conversion luminescence is characterized in that, comprises the steps:
Step S1, according to structural formula Y
2-x-yO
3: xHo
3+, yYb
3+In each element chemistry metering ratio, take by weighing powder: Y
2O
3, Ho
2O
3And Yb
2O
3
Step S2, the powder that step S1 is taken by weighing mix, ground 20～60 minutes, obtain the powder presoma;
Step S3, with the powder presoma of step S2 in 800～1000 ℃ of lower calcinings 0.5～5 hour, be cooled to subsequently 100～500 ℃, and after being incubated 0.5～3 hour under this temperature, be cooled to room temperature, obtain block product;
Step S4, the block product among the step S3 is ground, obtain the fluorescent material of described yttrium oxide up-conversion luminescence; The structural formula of this fluorescent material is Y
2-x-yO
3: xHo
3+, yYb
3+Wherein, Ho
3+And Yb
3+Be dopant ion; The span of x is that the span of 0.02～0.1, y is 0.02～0.2.
4. the preparation method of the fluorescent material of yttrium oxide up-conversion luminescence according to claim 3 is characterized in that, among the step S2, the milling time of described powder is 40 minutes.
5. the preparation method of the fluorescent material of yttrium oxide up-conversion luminescence according to claim 3 is characterized in that, among the step S3, the calcining temperature of described calcination process is 950 ℃, and calcination time is 3 hours.
6. the preparation method of the fluorescent material of yttrium oxide up-conversion luminescence according to claim 3 is characterized in that, among the step S3, after calcination process finished, the temperature of described insulating process was 250 ℃, and soaking time is 2 hours.
7. the preparation method of the fluorescent material of yttrium oxide up-conversion luminescence according to claim 3 is characterized in that, described structural formula Y
2-x-yO
3: xHo
3+, yYb
3+In, x value 0.06, y value 0.1.
8. the application of fluorescent material in Organic Light Emitting Diode of claim 1 or 2 described yttrium oxide up-conversion luminescences.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687306A (en) * | 2005-04-29 | 2005-10-26 | 中国科学院上海硅酸盐研究所 | Luminescent material converted in nano level with yttrium oxide as matrix and preparation method |
| CN101016459A (en) * | 2007-02-14 | 2007-08-15 | 湘潭大学 | White up conversion material and preparing method thereof |
| US20100124658A1 (en) * | 2005-09-29 | 2010-05-20 | Trustees Of Princeton University | Method for synthesizing phosphorescent oxide nanoparticles |
-
2011
- 2011-10-19 CN CN2011103203254A patent/CN103059855A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687306A (en) * | 2005-04-29 | 2005-10-26 | 中国科学院上海硅酸盐研究所 | Luminescent material converted in nano level with yttrium oxide as matrix and preparation method |
| US20100124658A1 (en) * | 2005-09-29 | 2010-05-20 | Trustees Of Princeton University | Method for synthesizing phosphorescent oxide nanoparticles |
| CN101016459A (en) * | 2007-02-14 | 2007-08-15 | 湘潭大学 | White up conversion material and preparing method thereof |
Non-Patent Citations (9)
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|---|
| J. A. CAPOBIANCO ET AL.: "Optical Spectroscopy and Upconversion Studies of Ho3+-Doped Bulk and Nanocrystalline Y2O3", 《CHEM. MATER.》 * |
| MINGMING XING ET AL.: "Synthesis and upconversion luminescence properties of monodisperse Y2O3:Yb,Ho spherical particles", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| YANPING LI ET AL.: "Near-Infrared to Visible Upconversion in Er3+ and Yb3+ Codoped Lu2O3 Nanocrystals: Enhanced Red Color Upconversion and Three-Photon Process in Green Color Upconversion", 《J. PHYS. CHEM. C》 * |
| 于晓波等: "Tm3+/Ho3+/Yb3+掺杂铋碲酸盐玻璃上转换白光", 《光学学报》 * |
| 张向华等: "980 nm激发下Ho3+/Yb3共掺杂ZrO2-ZnO粉末的上转换发光特性", 《光谱学与光谱分析》 * |
| 张向华等: "烧结温度对Er3+/Yb3+共掺氟氧化物粉末上转换发光的影响", 《硅酸盐通报》 * |
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Application publication date: 20130424 |