CN103059858B - Yttrium silicate upconversion luminous fluorescent powder, preparation method and application thereof - Google Patents
Yttrium silicate upconversion luminous fluorescent powder, preparation method and application thereof Download PDFInfo
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- CN103059858B CN103059858B CN201110318785.3A CN201110318785A CN103059858B CN 103059858 B CN103059858 B CN 103059858B CN 201110318785 A CN201110318785 A CN 201110318785A CN 103059858 B CN103059858 B CN 103059858B
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- yttrium silicate
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- conversion luminescence
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Abstract
The invention belongs to the field of fluorescent powder, and discloses an yttrium silicate upconversion luminous fluorescent powder, and a preparation method and application thereof. The fluorescent powder has a structure of Y2-xSiO5:xHo<3+>; Ho<3+> is a doping ion; and x is in the range from 0.02 to 0.1. The yttrium silicate upconversion luminous fluorescent powder prepared by the invention can realize blue short-wavelength light emitting through excitation by long-wave radiation from infrared to green ray. Therefore, the fluorescent powder can make up for the lack of blue material in current display and luminous material.
Description
Technical field
The present invention relates to a kind of fluorescent material, relate in particular to fluorescent material of a kind of yttrium silicate 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, more has flexible characteristic, makes its range of application extremely wide.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 be prepared into fluorescent material and be applied to the field of OLED, still rarely seen report.
Summary of the invention
One of object 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 silicate up-conversion luminescence of blue emission.
A fluorescent material for yttrium silicate up-conversion luminescence, its structural formula is Y
2-xsiO
5: xHo
3+; Wherein, Ho
3+for dopant ion, the span of x is 0.02～0.1; Preferably, x value 0.06.
The preparation method who another object of the present invention is to the fluorescent material that above-mentioned yttrium silicate up-conversion luminescence is provided, comprises the steps:
Step S1, according to structural formula Y
2-xsiO
5: xHo
3+in each element chemistry metering ratio, take powder: Y
2o
3, SiO
2and Ho
2o
3;
Step S2, the powder that step S1 is taken mix, grind 20～60 minutes, obtain powder presoma;
Step S3, the powder presoma of step S2 is calcined 0.5～5 hour at 800～1000 DEG C, be cooled to subsequently 100～500 DEG C, and be cooled to room temperature be incubated 0.5～3 hour at this temperature after, obtain block product;
Step S4, the block product in step S3 is ground, obtain the fluorescent material of described yttrium silicate up-conversion luminescence; The structural formula of this fluorescent material is Y
2-xsiO
5: xHo
3+; Wherein, Ho
3+for dopant ion;
Wherein, structural formula Y
2-xsiO
5: xHo
3+in, the span of x is 0.02～0.1.
In the preparation method of the fluorescent material of above-mentioned yttrium silicate up-conversion luminescence:
In step S2, the milling time of described powder is 40 minutes;
In step S3, the calcining temperature of described calcination process is 950 DEG C, and calcination time is 3 hours; After calcination process finishes, the temperature of described insulating process is 250 DEG C, and soaking time is 2 hours;
Structural formula Y
2-xsiO
5: xHo
3+in, preferably, x value 0.06.
The application of the fluorescent material that another object of the present invention is to provide above-mentioned yttrium silicate up-conversion luminescence in Organic Light Emitting Diode is mainly the luminescent layer material as Organic Light Emitting Diode.These fluorescent material are being, after the Organic Light Emitting Diode of carrying out monochrome (as ruddiness) is made, fluorescent material to be mixed in packaged material and to be coated in Organic Light Emitting Diode outside, are subject to exciting of ruddiness, give off blue light.
The fluorescent material of yttrium silicate up-conversion luminescence prepared by the present invention, can realize that to inspire blue light shortwave by the infrared long-wave radiation to green glow luminous.Therefore, this fluorescent material can make up the deficiency of blue light material in current demonstration and luminescent material.
In addition, the preparation method of the fluorescent material of yttrium silicate up-conversion luminescence provided by the invention is simple, is with low costly applicable to production, and reaction process, without three industrial wastes, belongs to environmental protection, less energy-consumption, high benefit industry.
Brief description of the drawings
Fig. 1 is preparation technology's schema of the fluorescent material of yttrium silicate up-conversion luminescence of the present invention;
Fig. 2 is the electroluminescent spectrum figure of the fluorescent material of the yttrium silicate up-conversion luminescence that makes of embodiment 1;
Fig. 3 is the structural representation of the Organic Light Emitting Diode of embodiment 4.
Embodiment
The fluorescent material of a kind of yttrium silicate up-conversion luminescence provided by the invention, its structural formula is Y
2-xsiO
5: xHo
3+; Wherein, Ho
3+for dopant ion, the span of x is 0.02～0.1; Preferably, x value 0.06.
The fluorescent material of yttrium silicate up-conversion luminescence prepared by the present invention, can realize that to inspire blue light shortwave by the infrared long-wave radiation to green glow luminous.Therefore, this fluorescent material can make up the deficiency of blue light material in current demonstration and luminescent material.
The preparation method of the fluorescent material of above-mentioned yttrium silicate up-conversion luminescence, as shown in Figure 1, comprises the steps:
Step S1, according to structural formula Y
2-xsiO
5: xHo
3+in each element chemistry metering ratio, take powder: Y
2o
3, SiO
2and Ho
2o
3;
Step S2, the powder that step S1 is taken mix, grind 20～60 minutes, obtain powder presoma;
Step S3, the powder presoma of step S2 is calcined 0.5～5 hour at 800～1000 DEG C, be cooled to subsequently 100～500 DEG C, and be cooled to room temperature be incubated 0.5～3 hour at this temperature after, obtain block product;
Step S4, the block product in step S3 is ground, obtain the fluorescent material of described yttrium silicate up-conversion luminescence; The structural formula of this fluorescent material is Y
2-xsiO
5: xHo
3+; Wherein, Ho
3+for dopant ion;
Wherein, structural formula Y
2-xsiO
5: xHo
3+in, the span of x is 0.02～0.1.
In the preparation method of the fluorescent material of above-mentioned yttrium silicate up-conversion luminescence:
In step S2, the milling time of described powder is 40 minutes;
In step S3, the calcining temperature of described calcination process is 950 DEG C, and calcination time is 3 hours; After calcination process finishes, the temperature of described insulating process is 250 DEG C, and soaking time is 2 hours;
Structural formula Y
2-xsiO
5: xHo
3+in, preferably, x value 0.06.
The preparation method of the fluorescent material of yttrium silicate up-conversion luminescence provided by the invention is simple, is with low costly applicable to production, and reaction process, without three industrial wastes, belongs to environmental protection, less energy-consumption, high benefit industry.
The application of the fluorescent material of above-mentioned yttrium silicate up-conversion luminescence in Organic Light Emitting Diode is mainly the luminescent layer material as Organic Light Emitting Diode.These fluorescent material are being, after the Organic Light Emitting Diode of carrying out monochrome (as ruddiness) is made, fluorescent material to be mixed in packaged material and to be coated in Organic Light Emitting Diode outside, 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, SiO
2and Ho
2o
3powder, its quality is respectively 0.37g, 0.8g and 0.113g;
2, above-mentioned powder is placed in to corundum mortar, grinds and it was evenly mixed in 40 minutes, obtain powder presoma;
3, powder presoma is placed in to retort furnace, calcination 3 hours at 950 DEG C, is then cooled to 250 DEG C of insulations 3 hours, then naturally cools to room temperature taking-up block product,
4, block product is ground, pulverized, obtaining structural formula is Y
1.94siO
5: 0.06Ho
3+up-conversion phosphor.
Fig. 2 is the electroluminescent spectrum figure of the fluorescent material of the yttrium silicate up-conversion luminescence that makes of embodiment 1; As shown in Figure 2, excitation wavelength is 640nm, and that the glow peak of the 490nm obtaining is corresponding is Ho
3+ion
5f
3→
51
8transition radiation luminous.
Embodiment 2
1, selecting purity is 99.99% powder: Y
2o
3, SiO
2and Ho
2o
3powder, its mass ratio is respectively 2.32g, 0.8g and 0.150g;
2, above-mentioned powder is placed in to corundum mortar and grinds and it was evenly mixed in 20 minutes, obtain powder presoma;
3, powder presoma is placed in to retort furnace, calcination 5 hours at 800 DEG C, is then cooled to 100 DEG C of insulations 3 hours, then naturally cools to room temperature taking-up block product;
4, block product is ground, pulverized, obtaining structural formula is Y
1.9siO
5: 0.1Ho
3+up-conversion phosphor.
Embodiment 3
1, selecting purity is 99.99% powder: Y
2o
3, SiO
2and Ho
2o
3powder, its quality is respectively 2.42g, 0.8g and 0.038g;
2, above-mentioned powder is placed in to corundum mortar and grinds and it was evenly mixed in 60 minutes, obtain powder presoma;
3, powder presoma is placed in to retort furnace, calcination 0.5 hour at 1000 DEG C, is then cooled to 500 DEG C of insulations 0.5 hour, then naturally cools to room temperature taking-up block product;
4, block product is ground, pulverized, obtaining structural formula is Y
1.98siO
5: 0.02Ho
3+up-conversion phosphor.
Embodiment 4
The present embodiment 4 is Organic Light Emitting Diode, refers to 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 stacking gradually; Wherein, in transparent encapsulated layer 5, be dispersed with the fluorescent material 6 making in embodiment 1.
When this Organic Light Emitting Diode uses, the part ruddiness excitated fluorescent powder 6 of organic luminous layer 3 sends blue light, and this blue light inspires white light after mixing with remaining ruddiness in luminescent layer 3.
Should be understood that, the 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 (6)
1. a fluorescent material for yttrium silicate up-conversion luminescence, is characterized in that, the structural formula of this fluorescent material is Y
2-xsiO
5: xHo
3+; Wherein, Ho
3+for dopant ion, the span of x is 0.02～0.1.
2. the fluorescent material of yttrium silicate up-conversion luminescence according to claim 1, is characterized in that, x value 0.06.
3. a preparation method for the fluorescent material of yttrium silicate up-conversion luminescence, is characterized in that, comprises the steps:
Step S1, according to structural formula Y
2-xsiO
5: xHo
3+in each element chemistry metering ratio, take powder: Y
2o
3, SiO
2and Ho
2o
3;
Step S2, the powder that step S1 is taken mix, grind 20～60 minutes, obtain powder presoma;
Step S3, the powder presoma of step S2 is calcined 3 hours at 950 DEG C, be cooled to subsequently 250 DEG C, and be cooled to room temperature be incubated 2 hours at this temperature after, obtain block product;
Step S4, the block product in step S3 is ground, obtain the fluorescent material of described yttrium silicate up-conversion luminescence; The structural formula of this fluorescent material is Y
2-xsiO
5: xHo
3+; Wherein, Ho
3+for dopant ion;
Wherein, structural formula Y
2-xsiO
5: xHo
3+in, the span of x is 0.02～0.1.
4. the preparation method of the fluorescent material of yttrium silicate up-conversion luminescence according to claim 3, is characterized in that, in step S2, the milling time of described powder is 40 minutes.
5. the preparation method of the fluorescent material of yttrium silicate up-conversion luminescence according to claim 3, is characterized in that, described structural formula Y
2-xsiO
5: xHo
3+in, x value 0.06.
6. the application of the fluorescent material of yttrium silicate up-conversion luminescence in Organic Light Emitting Diode described in claim 1 or 2.
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| CN201110318785.3A CN103059858B (en) | 2011-10-19 | 2011-10-19 | Yttrium silicate upconversion luminous fluorescent powder, preparation method and application thereof |
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| CN103059858B true CN103059858B (en) | 2014-10-01 |
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| WO2016203431A1 (en) | 2015-06-18 | 2016-12-22 | Universita' Ca' Foscari | Luminescent bismuth silicates, use and method for producing thereof |
| CN110092649B (en) * | 2018-01-31 | 2021-07-23 | 中国科学院金属研究所 | Yttrium holmium monosilicate solid solution material and preparation method thereof |
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| US6762875B2 (en) * | 2002-02-07 | 2004-07-13 | Corning Incorporated | Creating refractive index changes in glass by up-conversion of rare earth ions |
| JP3872472B2 (en) * | 2003-11-12 | 2007-01-24 | 日亜化学工業株式会社 | Green light emitting yttrium silicate phosphor for projection tube and projection tube using the same |
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