CN103059867B - Tellurate phosphors for up-conversion luminescence, and preparation method and application thereof - Google Patents
Tellurate phosphors for up-conversion luminescence, and preparation method and application thereof Download PDFInfo
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- CN103059867B CN103059867B CN201110320306.1A CN201110320306A CN103059867B CN 103059867 B CN103059867 B CN 103059867B CN 201110320306 A CN201110320306 A CN 201110320306A CN 103059867 B CN103059867 B CN 103059867B
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- tellurate
- fluorescent material
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- conversion luminescence
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Abstract
The invention belongs to the phosphor field, and discloses tellurate phosphors for up-conversion luminescence, and a preparation method and an application thereof. The phosphors have a structural formula of aTeO2-bTiO2-cLa2O3:dTb3+, wherein Tb3+ is doping ions; a, b, c and d represent molar coefficients; a is equal to or greater than 0.85 and less than or equal to 0.92; b is equal to or greater than 0.01 and less than or equal to 0.08; c is equal to or greater than 0.01 and less than or equal to 0.08; d is equal to or greater than 0.005 and less than or equal to 0.05; and a sum of a, b, c and d is equal to 1. The tellurate 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, particularly relate to fluorescent material of a kind of tellurate 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 have flexible characteristic, makes its range of application extremely wide.But because the OLED blue light material obtaining stability and high efficiency is at present more difficult, significantly limit the development of white light OLED device and light source industry.
Upconverting fluorescent material can launch visible ray under long wave (as infrared) radiation excitation, even UV-light, is with a wide range of applications in the field such as optical fiber communication technology, fibre amplifier, 3 D stereo display, biomolecules fluorescence labelling, infrared detective.But be prepared into the field that fluorescent material is applied to OLED, still rarely seen report.
Summary of the invention
An object of the present invention is to provide a kind of fluorescent material that can be inspired the tellurate up-conversion luminescence of blue emission by long wavelength radiations such as infrared, red-green glows.
A fluorescent material for tellurate up-conversion luminescence, its structural formula is aTeO
2-bTiO
2-cLa
2o
3: dTb
3+; Wherein, Tb
3+for dopant ion, a, b, c, d are mole coefficient, 0.85≤a≤0.92,0.01≤b≤0.08,0.01≤c≤0.08,0.005≤d≤0.05, and a+b+c+d=1; Preferably, a=0.88, b=0.05, c=0.05, d=0.02.
Another object of the present invention is to the preparation method of the fluorescent material that above-mentioned tellurate up-conversion luminescence is provided, comprise the steps:
Step S1, according to molecular fraction, take powder: TeO
2, 85% ~ 92%; TiO
2, 1% ~ 8%; La
2o
3, 1% ~ 8%; Tb
2o
3, 0.5% ~ 5%;
Step S2, the powder taken by step S1 mix, grind 20 ~ 60 minutes, obtain powder presoma;
Step S3, the powder presoma of step S2 to be calcined 0.5 ~ 5 hour at 900 ~ 1100 DEG C, be cooled to 100 ~ 300 DEG C subsequently, and be cooled to room temperature after being incubated 0.5 ~ 3 hour at this temperature, obtain block product;
Step S4, the block product in step S3 to be ground, obtain the fluorescent material of described tellurate up-conversion luminescence; The structural formula of this fluorescent material is aTeO
2-bTiO
2-cLa
2o
3: dTb
3+; Wherein, Tb
3+for dopant ion, a, b, c, d are mole coefficient, 0.85≤a≤0.92,0.01≤b≤0.08,0.01≤c≤0.08,0.005≤d≤0.05, and a+b+c+d=1.
In the preparation method of the fluorescent material of above-mentioned tellurate up-conversion luminescence:
In step S1, preferably, a=0.88, b=0.05, c=0.05, d=0.02;
In step S2, the milling time of described powder is 40 minutes;
In step S3, the calcining temperature of described calcination process is 1000 DEG C, and calcination time is 3 hours; After calcination process terminates, the temperature of described insulating process is 200 DEG C, and soaking time is 2 hours.
Another object of the present invention is the application of fluorescent material in Organic Light Emitting Diode providing above-mentioned tellurate up-conversion luminescence, is mainly used as the emitting layer material of Organic Light Emitting Diode.These fluorescent material are being, after the Organic Light Emitting Diode carrying out monochrome (as ruddiness) is made, fluorescent material is mixed in packaged material and is coated in outside Organic Light Emitting Diode, be subject to exciting of ruddiness, give off blue light.
The fluorescent material of tellurate up-conversion luminescence prepared by the present invention, can realize inspiring 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 display at present and luminescent material.
In addition, the preparation method of the fluorescent material of tellurate 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.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of the fluorescent material of tellurate up-conversion luminescence of the present invention;
Fig. 2 is the electroluminescent spectrum figure of the fluorescent material of the tellurate up-conversion luminescence that embodiment 1 obtains;
Fig. 3 is the organic LED structure schematic diagram of embodiment 4.
Embodiment
The fluorescent material of a kind of tellurate up-conversion luminescence provided by the invention, its structural formula is aTeO
2-bTiO
2-cLa
2o
3: dTb
3+; Wherein, Tb
3+for dopant ion, aTeO
2-bTiO
2-cLa
2o
3system be that one can allow Tb
3+realize the matrix of transform light energy, a, b, c, d are mole coefficient, 0.85≤a≤0.92,0.01≤b≤0.08,0.01≤c≤0.08,0.005≤d≤0.05, and a+b+c+d=1; Preferably, a=0.88, b=0.05, c=0.05, d=0.02.
The fluorescent material of tellurate up-conversion luminescence prepared by the present invention, can realize inspiring 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 display at present and luminescent material.
The preparation method of the fluorescent material of above-mentioned tellurate up-conversion luminescence, as shown in Figure 1, comprises the steps:
Step S1, according to molecular fraction, take powder: TeO
2, 85% ~ 92%; TiO
2, 1% ~ 8%; La
2o
3, 1% ~ 8%; Tb
2o
3, 0.5% ~ 5%;
Step S2, the powder taken by step S1 mix, grind 20 ~ 60 minutes, obtain powder presoma;
Step S3, the powder presoma of step S2 to be calcined 0.5 ~ 5 hour at 900 ~ 1100 DEG C, be cooled to 100 ~ 300 DEG C subsequently, and be cooled to room temperature after being incubated 0.5 ~ 3 hour at this temperature, obtain block product;
Step S4, the block product in step S3 to be ground, obtain the fluorescent material of described tellurate up-conversion luminescence; The structural formula of this fluorescent material is aTeO
2-bTiO
2-cLa
2o
3: dTb
3+; Wherein, Tb
3+for dopant ion, a, b, c, d are mole coefficient, 0.85≤a≤0.92,0.01≤b≤0.08,0.01≤c≤0.08,0.005≤d≤0.05, and a+b+c+d=1.
In the preparation method of the fluorescent material of above-mentioned tellurate up-conversion luminescence:
In step S1, preferably, a=0.88, b=0.05, c=0.05, d=0.02;
In step S2, the milling time of described powder is 40 minutes;
In step S3, the calcining temperature of described calcination process is 1000 DEG C, and calcination time is 3 hours; After calcination process terminates, the temperature of described insulating process is 200 DEG C, and soaking time is 2 hours.
The preparation method of the fluorescent material of tellurate 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 fluorescent material in Organic Light Emitting Diode of above-mentioned tellurate up-conversion luminescence, is mainly used as the emitting layer material of Organic Light Emitting Diode.These fluorescent material are being, after the Organic Light Emitting Diode carrying out monochrome (as ruddiness) is made, fluorescent material is mixed in packaged material and is coated in outside Organic Light Emitting Diode, be 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, select purity be 99.99% powder: TeO
2, TiO
2, La
2o
3and Tb
2o
3powder, its mole hundred number is respectively 88%, 5%, 5% and 2%;
2, above-mentioned powder is placed in corundum mortar, grinds and make its Homogeneous phase mixing in 40 minutes, obtain powder presoma;
3, powder presoma is placed in retort furnace, calcination 3 hours at 1000 DEG C, is then cooled to 200 DEG C to be incubated 2 hours, then naturally cool to room temperature taking-up block product,
4, ground by block product, pulverize, obtaining structural formula is 0.88TeO
2-0.05TiO
2-0.05La
2o
3: 0.02Tb
3+up-conversion phosphor.
Fig. 2 is the electroluminescent spectrum figure of the fluorescent material of the tellurate up-conversion luminescence that embodiment 1 obtains; As shown in Figure 2, excitation wavelength is 796nm; That the glow peak of the 485nm obtained is corresponding is Tb
3+ion
5d
4→
7f
6transition radiation luminous.
Embodiment 2
1, select purity be 99.99% powder: TeO
2, TiO
2, La
2o
3and Tb
2o
3powder, its molecular fraction is respectively 92%, 1%, 2% and 5%;
2, above-mentioned powder is placed in the grinding of corundum mortar and makes its Homogeneous phase mixing in 20 minutes, obtain powder presoma;
3, powder presoma is placed in retort furnace, calcination 5 hours at 900 DEG C, is then cooled to 300 DEG C to be incubated 0.5 hour, then naturally cool to room temperature taking-up block product;
4, ground by block product, pulverize, obtaining structural formula is 0.92TeO
2-0.01TiO
2-0.02La
2o
3: 0.05Tb
3+up-conversion phosphor.
Embodiment 3
1, select purity be 99.99% powder: TeO
2, TiO
2, La
2o
3and Tb
2o
3powder, its molecular fraction is respectively 85%, 8%, 6.5% and 0.5%;
2, above-mentioned powder is placed in the grinding of corundum mortar and makes its Homogeneous phase mixing in 60 minutes, obtain powder presoma;
3, powder presoma is placed in retort furnace, calcination 0.5 hour at 1100 DEG C, is then cooled to 100 DEG C to be incubated 3 hours, then naturally cool to room temperature taking-up block product;
4, ground by block product, pulverize, obtaining structural formula is 0.85TeO
2-0.08TiO
2-0.065La
2o
3: 0.005Tb
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 the substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the transparent encapsulated layer 5 that stack gradually; Wherein, fluorescent material 6 obtained in embodiment 1 is dispersed with in transparent encapsulated layer 5.
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 present pre-ferred embodiments is comparatively detailed, and therefore can not think the restriction to scope of patent protection of the present invention, scope of patent protection of the present invention should be as the criterion with claims.
Claims (3)
1. a preparation method for the fluorescent material of tellurate up-conversion luminescence, is characterized in that, comprises the steps:
Step S1, according to molecular fraction, take powder: TeO
2, 85% ~ 92%; TiO
2, 1% ~ 8%; La
2o
3, 1% ~ 8%; Tb
2o
3, 0.5% ~ 5%;
Step S2, the powder taken by step S1 mix, grind 20 ~ 60 minutes, obtain powder presoma;
Step S3, the powder presoma of step S2 to be calcined 3 hours at 1000 DEG C, be cooled to 200 DEG C subsequently, and be cooled to room temperature after being incubated 2 hours at this temperature, obtain block product;
Step S4, the block product in step S3 to be ground, obtain the fluorescent material of described tellurate up-conversion luminescence; The structural formula of this fluorescent material is aTeO
2-bTiO
2-cLa
2o
3: dTb
3+; Wherein, Tb
3+for dopant ion, a, b, c, d are mole coefficient, 0.85≤a≤0.92,0.01≤b≤0.08,0.01≤c≤0.08,0.005≤d≤0.05, and a+b+c+d=1.
2. the preparation method of the fluorescent material of tellurate up-conversion luminescence according to claim 1, is characterized in that, in step S4, and a=0.88, b=0.05, c=0.05, d=0.02.
3. the preparation method of the fluorescent material of tellurate up-conversion luminescence according to claim 1, is characterized in that, in step S2, the milling time of described powder is 40 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110320306.1A CN103059867B (en) | 2011-10-19 | 2011-10-19 | Tellurate phosphors for up-conversion luminescence, and preparation method and application thereof |
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|---|---|---|---|
| CN201110320306.1A CN103059867B (en) | 2011-10-19 | 2011-10-19 | Tellurate phosphors for up-conversion luminescence, and preparation method and application thereof |
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| CN103059867B true CN103059867B (en) | 2015-04-01 |
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ID=48102775
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201110320306.1A Active CN103059867B (en) | 2011-10-19 | 2011-10-19 | Tellurate phosphors for up-conversion luminescence, and preparation method and application thereof |
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| Country | Link |
|---|---|
| CN (1) | CN103059867B (en) |
-
2011
- 2011-10-19 CN CN201110320306.1A patent/CN103059867B/en active Active
Non-Patent Citations (4)
| Title |
|---|
| MA Hongping et al..Three-photon-excited fluorescence of Tb3+-doped CaO-Al2O3-SiO2 glass by femtosecond laser irradiation.《JOURNAL OF RARE EARTHS》.2008, * |
| TranKim Anh et al..Luminescence, Energy Transfer, and Upconversion Mechanisms of Y2O3 Nanomaterials Doped with Eu3+, Tb3+, Tm3+, Er3+, and Yb3+ Ions.《Journal of Nanomaterials》.2007, * |
| W. Stambouli et al..Energy transfer induced Eu3+ photoluminescence enhancement in tellurite glass.《Journal of Luminescence》.2011, * |
| Zhang Jihong et al..Structure, Upconversion and Fluorescence Properties of Er3+-Doped TeO2-TiO2-La2O3 Tellurite Glass.《Journal of Rare Earths》.2007, * |
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|---|---|
| CN103059867A (en) | 2013-04-24 |
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