CN103059865A - Oxyfluoride silicate upconversion luminous fluorescent powder, preparation method and application thereof - Google Patents
Oxyfluoride silicate upconversion luminous fluorescent powder, preparation method and application thereof Download PDFInfo
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- CN103059865A CN103059865A CN2011103187745A CN201110318774A CN103059865A CN 103059865 A CN103059865 A CN 103059865A CN 2011103187745 A CN2011103187745 A CN 2011103187745A CN 201110318774 A CN201110318774 A CN 201110318774A CN 103059865 A CN103059865 A CN 103059865A
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Abstract
The invention belongs to the field of fluorescent powder, and discloses an oxyfluoride silicate upconversion fluorescent powder, and a preparation method and application thereof. The fluorescent powder has a structure of aNa2O-bLaF3-cAl2O3-dSiO2:eTm<3+>; Tm<3+> is a doping ion; and a, b, c, d and e represent molar coefficients, and satisfy the following relations: 0.08<=a<=0.13, 0.06<=b<=0.115, 0.25<=c<=0.32, 0.48<=d<=0.53, 0.005<=e<=0.03, and a+b+c+d+e=1. The oxyfluoride silicate upconversion fluorescence 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 fluorine oxygen 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, 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 fluorine oxygen silicate up-conversion luminescence of blue emission.
The fluorescent material of a kind of fluorine oxygen silicate up-conversion luminescence, its structural formula is aNa
2O-bLaF
3-cAl
2O
3-dSiO
2: eTm
3+Wherein, Tm
3+Be dopant ion, a, b, c, d, e are mole coefficient, 0.08≤a≤0.13,0.06≤b≤0.115,0.25≤c≤0.32,0.48≤d≤0.53,0.005≤e≤0.03, and a+b+c+d+e=1; Preferably, a=0.11, b=0.09, c=0.29, d=0.5, e=0.01.
Another object of the present invention is to provide the preparation method of the fluorescent material of above-mentioned fluorine oxygen silicate up-conversion luminescence, comprise the steps:
Step S1, according to molecular fraction, take by weighing powder: Na
2CO
3, 8～13%; LaF
3, 6～11.5%; Al
2O
3, 25～32%; SiO
2, 48～53%; Tm
2O
3, 0.5～3%;
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 900～1400 ℃ of lower calcinings 0.5～5 hour, be cooled to subsequently 600～800 ℃, 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 fluorine oxygen silicate up-conversion luminescence; The structural formula of this fluorescent material is aNa
2O-bLaF
3-cAl
2O
3-dSiO
2: eTm
3+Wherein, Tm
3+Be dopant ion, a, b, c, d, e are mole coefficient, 0.08≤a≤0.13,0.06≤b≤0.115,0.25≤c≤0.32,0.48≤d≤0.53,0.005≤e≤0.03, and a+b+c+d+e=1.
Among the preparation method of the fluorescent material of above-mentioned fluorine oxygen silicate up-conversion luminescence:
Among the step S1, preferred, a=0.11, b=0.09, c=0.29, d=0.5, e=0.01;
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 1200 ℃, and calcination time is 3 hours; After calcination process finished, the temperature of described insulating process was 700 ℃, and soaking time is 2 hours.
Another purpose of the present invention is to provide the application of fluorescent material in Organic Light Emitting Diode of above-mentioned fluorine oxygen silicate 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 fluorine oxygen silicate up-conversion luminescence of the present invention's preparation, it is luminous to realize inspiring the blue light shortwave by infrared long-wave radiation to green glow.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 fluorine oxygen silicate provided by the invention up-conversion luminescence 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 fluorine oxygen silicate of the present invention up-conversion luminescence;
Fig. 2 is the fluorescent material of the fluorine oxygen silicate up-conversion luminescence that makes of embodiment 1 and the electroluminescent spectrum figure of the fluorescent material of doped with fluorine oxygen silicate up-conversion luminescence not.
Fig. 3 is the structural representation of the Organic Light Emitting Diode of embodiment 4.
Embodiment
The fluorescent material of a kind of fluorine oxygen silicate provided by the invention up-conversion luminescence, its structural formula is aNa
2O-bLaF
3-cAl
2O
3-dSiO
2: eTm
3+Wherein, Tm
3+Be dopant ion, Na
2O-LaF
3-Al
2O
3-SiO
2System is a kind of matrix that can make ion generation transform light energy.A, b, c, d, e are mole coefficient, 0.08≤a≤0.13,0.06≤b≤0.115,0.25≤c≤0.32,0.48≤d≤0.53,0.005≤e≤0.03, and a+b+c+d+e=1; Preferably, a=0.11, b=0.09, c=0.29, d=0.5, e=0.01.
The fluorescent material of the fluorine oxygen silicate up-conversion luminescence of the present invention's preparation, it is luminous to realize inspiring the blue light shortwave by infrared long-wave radiation to green glow.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 fluorine oxygen silicate up-conversion luminescence as shown in Figure 1, comprises the steps:
Step S1, according to molecular fraction, take by weighing powder: Na
2CO
3, 8～13%; LaF
3, 6～11.5%; Al
2O
3, 25～32%; SiO
2, 48～53%; Tm
2O
3, 0.5～3%;
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 900～1400 ℃ of lower calcinings 0.5～5 hour, be cooled to subsequently 600～800 ℃, 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 fluorine oxygen silicate up-conversion luminescence; The structural formula of this fluorescent material is aNa
2O-bLaF
3-cAl
2O
3-dSiO
2: eTm
3+Wherein, Tm
3+Be dopant ion, a, b, c, d, e are mole coefficient, 0.08≤a≤0.13,0.06≤b≤0.115,0.25≤c≤0.32,0.48≤d≤053,0.005≤e≤003, and a+b+c+d+e=1.
Among the preparation method of the fluorescent material of above-mentioned fluorine oxygen silicate up-conversion luminescence:
Among the step S1, preferred, a=0.11, b=0.09, c=0.29, d=0.5, e=0.01;
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 1200 ℃, and calcination time is 3 hours; After calcination process finished, the temperature of described insulating process was 700 ℃, and soaking time is 2 hours.
Another purpose of the present invention is to provide the application of fluorescent material in Organic Light Emitting Diode of above-mentioned fluorine oxygen silicate 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.
In addition, the preparation method of the fluorescent material of fluorine oxygen silicate provided by the invention up-conversion luminescence 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.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
1, selecting purity is 99.99% powder: Na
2CO
3, LaF
3, Al
2O
3, SiO
2And Tm
2O
3Powder, its molecular fraction is respectively 11%, 9%, 29%, 50% and 1%;
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, 1200 ℃ of lower calcinations 3 hours, then is cooled to 700 ℃ of insulations 2 hours, naturally cool to again room temperature and take out block product,
4, block product is ground, pulverizes, obtaining structural formula is 0.11Na
2O-0.09LaF
3-0.29Al
2O
3-0.5SiO
2: 0.01Tm
3+Up-conversion phosphor.
Fig. 2 is the electroluminescent spectrum figure of the fluorescent material of the fluorine oxygen silicate up-conversion luminescence that makes of embodiment 1; Shown in Figure 2, excitation wavelength is 796nm; Wherein, the glow peak of 475nm is corresponding respectively is Tm
3+Ion
1G
4→
3H
6Transition radiation luminous.
1, selecting purity is 99.99% powder: Na
2CO
3, LaF
3, Al
2O
3, SiO
2And Tm
2O
3Powder, its molecular fraction is respectively 8%, 11.5%, 32%, 48% and 0.5%;
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, 900 ℃ of lower calcinations 5 hours, then be cooled to 600 ℃ 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 0.08Na
2O-0.115LaF
3-0.32Al
2O
3-0.48SiO
2: 0.005Tm
3+Up-conversion phosphor.
1, selecting purity is 99.99% powder: Na
2CO
3, LaF
3, Al
2O
3, SiO
2And Tm
2O
3Powder, its molecular fraction is respectively 13%, 6%, 25%, 53% and 3%;
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, 1400 ℃ of lower calcinations 0.5 hour, then be cooled to 800 ℃ 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 Na
0.26La
0.06Al
0.5Si
0.53O
2.03F
0.12: 0.03Tm
3+Up-conversion phosphor.
Embodiment 4
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, scope of patent protection of the present invention should be as the criterion with claims.
Claims (8)
1. the fluorescent material of fluorine oxygen silicate up-conversion luminescence is characterized in that, the structural formula of this fluorescent material is aNa
2O-bLaF
3-cAl
2O
3-dSiO
2: eTm
3+Wherein, Tm
3+Be dopant ion, a, b, c, d, e are mole coefficient, 0.08≤a≤0.13,0.06≤b≤0.115,0.25≤c≤0.32,0.48≤d≤0.53,0.005≤e≤0.03, and a+b+c+d+e=1.
2. the fluorescent material of fluorine oxygen silicate according to claim 1 up-conversion luminescence is characterized in that a=0.11, b=0.09, c=0.29, d=0.5, e=0.01.
3. the preparation method of the fluorescent material of fluorine oxygen silicate up-conversion luminescence is characterized in that, comprises the steps:
Step S1, according to molecular fraction, take by weighing powder: Na
2CO
3, 8～13%; LaF
3, 6～11.5%; Al
2O
3, 25～32%; SiO
2, 48～53%; Tm
2O
3, 0.5～3%;
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 900～1400 ℃ of lower calcinings 0.5～5 hour, be cooled to subsequently 600～800 ℃, 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 fluorine oxygen silicate up-conversion luminescence; The structural formula of this fluorescent material is aNa
2O-bLaF
3-cAl
2O
3-dSiO
2: eTm
3+Wherein, Tm
3+Be dopant ion, a, b, c, d, e are mole coefficient, 0.08≤a≤0.13,0.06≤b≤0.115,0.25≤c≤0.32,0.48≤d≤0.53,0.005≤e≤0.03, and a+b+c+d+e=1.
4. the preparation method of the fluorescent material of fluorine oxygen silicate according to claim 3 up-conversion luminescence is characterized in that, among the step S1, and a=0.11, b=0.09, c=0.29, d=0.5, e=0.01.
5. the preparation method of the fluorescent material of fluorine oxygen silicate according to claim 3 up-conversion luminescence is characterized in that, among the step S2, the milling time of described powder is 40 minutes.
6. the preparation method of the fluorescent material of fluorine oxygen silicate according to claim 3 up-conversion luminescence is characterized in that, among the step S3, the calcining temperature of described calcination process is 1200 ℃, and calcination time is 3 hours.
7. the preparation method of the fluorescent material of fluorine oxygen silicate according to claim 3 up-conversion luminescence is characterized in that, among the step S3, after calcination process finished, the temperature of described insulating process was 700 ℃, and soaking time is 2 hours.
8. the application of fluorescent material in Organic Light Emitting Diode of claim 1 or 2 described fluorine oxygen silicate up-conversion luminescences.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104119919A (en) * | 2013-04-26 | 2014-10-29 | 海洋王照明科技股份有限公司 | Samarium-doped fluorine-containing aluminosilicate luminescent material and preparation method and application thereof |
| US9335011B2 (en) | 2014-07-02 | 2016-05-10 | General Electric Company | Oxyfluoride phosphor compositions and lighting apparatus thereof |
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2011
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104119919A (en) * | 2013-04-26 | 2014-10-29 | 海洋王照明科技股份有限公司 | Samarium-doped fluorine-containing aluminosilicate luminescent material and preparation method and application thereof |
| US9335011B2 (en) | 2014-07-02 | 2016-05-10 | General Electric Company | Oxyfluoride phosphor compositions and lighting apparatus thereof |
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