CN103045244B - Dysprosium doped barium titanium glass up-conversion luminescent material, preparation method and application thereof - Google Patents
Dysprosium doped barium titanium glass up-conversion luminescent material, preparation method and application thereof Download PDFInfo
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- CN103045244B CN103045244B CN201110314959.9A CN201110314959A CN103045244B CN 103045244 B CN103045244 B CN 103045244B CN 201110314959 A CN201110314959 A CN 201110314959A CN 103045244 B CN103045244 B CN 103045244B
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- luminescent material
- conversion luminescent
- dysprosium doped
- doped titanium
- barium glass
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Abstract
The invention discloses a dysprosium doped barium titanium glass up-conversion luminescent material with a chemical formula of aTiO2-bBaO-cB2O3-dSiO2:xDy<3+>, wherein a is 0.3-0.4, b is 0.2-0.3, c is 0.1-0.2, d is 0.2-0.3, and x is 0.001-0.01. In photoluminescence spectra of the dysprosium doped barium titanium glass up-conversion luminescent material, the excitation wavelength of the dysprosium doped barium titanium glass up-conversion luminescent material is 796nm, transition radiation of Dy<3+> ion 4F9/2->6F15/2 in a 482nm wavelength region forms a luminescent peak, and thus blue light short wave luminescence is excited by long-wave radiation from infrared light to green light. The invention also provides a preparation method of the dysprosium doped barium titanium glass up-conversion luminescent material, and an organic light emitting diode using the dysprosium doped barium titanium glass up-conversion luminescent material.
Description
[technical field]
The present invention relates to a kind of dysprosium doped titanium barium glass 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 is short, flexible, and obtain a very wide range of application.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, can by infrared, the long-wave radiations such as red-green glow inspire the dysprosium doped titanium barium glass 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 inspire the dysprosium doped titanium barium glass up-conversion luminescent material of blue light, preparation method by long-wave radiation and use the Organic Light Emitting Diode of this dysprosium doped titanium barium glass up-conversion luminescent material.
A kind of dysprosium doped titanium barium glass up-conversion luminescent material, its chemical formula is aTiO
2-bBaO-cB
2o
3-dSiO
2: xDy
3+, wherein, a is 0.3 ~ 0.4, b be 0.2 ~ 0.3, c be 0.1 ~ 0.2, d be 0.2 ~ 0.3, x is 0.001 ~ 0.01.
In a preferred embodiment, a is 0.35, b be 0.25, c be 0.16, d be 0.25, x is 0.08.
A preparation method for dysprosium doped titanium barium glass up-conversion luminescent material, comprises the following steps: step one, according to TiO
2, BaCO
3, H
3bO
3, SiO
2and Dy
2o
3each powder is (32 ~ 40) in molar ratio: (22 ~ 30): (10 ~ 16): (20 ~ 30): (0.1 ~ 1.5);
Step 2, the powder taken mixed obtain presoma in step one;
Step 3, by the calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C of described presoma, be cooled to 100 DEG C ~ 300 DEG C afterwards, then be incubated 0.5 hour ~ 3 hours and obtain dysprosium doped titanium barium glass up-conversion luminescent material, wherein chemical formula is aTiO
2-bBaO-cB
2o
3-dSiO
2: xDy
3+, wherein, a is 0.3 ~ 0.4, b be 0.2 ~ 0.3, c be 0.1 ~ 0.2, d be 0.2 ~ 0.3, x is 0.001 ~ 0.01.
In a preferred embodiment, a is 0.35, b be 0.25, c be 0.16, d be 0.25, x is 0.08.
In a preferred embodiment, in step 2, powder is ground 20 minutes ~ 60 minutes in corundum alms bowl body.
In a preferred embodiment, in step 3 by the calcination 3 hours at 950 DEG C of described presoma.
In a preferred embodiment, by the calcination 3 hours at 950 DEG C of described presoma in step 3, be cooled to 200 DEG C afterwards, then be incubated 2 hours and obtain dysprosium doped titanium barium glass up-conversion luminescent material.
In a preferred embodiment, the calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C of presoma described in step 3, be cooled to 100 DEG C ~ 300 DEG C afterwards, then after being incubated 0.5 hour ~ 3 hours, furnace cooling obtains bulk material to room temperature, described bulk material is pulverized and obtains target product.
In a preferred embodiment, in step 2, the powder ball milling taken is obtained the presoma mixed in step one.
A kind of Organic Light Emitting Diode, this Organic Light Emitting Diode comprises the negative electrode, luminescent layer, conductive layer and the anode that stack gradually, the material of described luminescent layer is dysprosium doped titanium barium glass up-conversion luminescent material, and the chemical formula of this dysprosium doped titanium barium glass up-conversion luminescent material is aTiO
2-bBaO-cB
2o
3-dSiO
2: xDy
3+, wherein, a is 0.3 ~ 0.4, b be 0.2 ~ 0.3, c be 0.1 ~ 0.2, d be 0.2 ~ 0.3, x is 0.001 ~ 0.01.
The preparation method of above-mentioned dysprosium doped titanium barium glass 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 the dysprosium doped titanium barium glass up-conversion luminescent material of preparation, the excitation wavelength of dysprosium doped titanium barium glass up-conversion luminescent material is 796nm, in 482nm wavelength zone by Dy
3+ion
4f
9/2→
6f
15/2transition radiation form glow peak, achieve that to inspire blue light shortwave by the infrared long-wave radiation to green glow luminous.
[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 dysprosium doped titanium barium glass up-conversion luminescent material prepared by embodiment 1.
[embodiment]
Below in conjunction with the drawings and specific embodiments, dysprosium doped titanium barium glass up-conversion luminescent material and preparation method thereof is illustrated further.
The dysprosium doped titanium barium glass up-conversion luminescent material of one embodiment, its chemical formula is aTiO
2-bBaO-cB
2o
3-dSiO
2: xDy
3+, wherein, a is 0.3 ~ 0.4, b be 0.2 ~ 0.3, c be 0.1 ~ 0.2, d be 0.2 ~ 0.3, x is 0.001 ~ 0.01.
Preferably, a is 0.35, b be 0.25, c be 0.16, d be 0.25, x is 0.08.
In the photoluminescence spectra of this dysprosium doped titanium barium glass up-conversion luminescent material, the excitation wavelength of dysprosium doped titanium barium glass up-conversion luminescent material is 796nm, when material is subject to the radiation of long wavelength (as 796nm) time, and Dy
3+the energy of this illumination of ionic absorption, now Dy
3+ion has just been in
4f
9/2excited state, then to
6f
15/2transition, just sends the blue light of 482nm, achieves and inspires the luminescence of blue light shortwave by the infrared long-wave radiation to green glow.
The preparation method of above-mentioned dysprosium doped titanium barium glass up-conversion luminescent material, comprises the following steps:
Step S11, according to TiO
2, BaCO
3, H
3bO
3, SiO
2and Dy
2o
3each powder is (32 ~ 40) in molar ratio: (22 ~ 30): (10 ~ 16): (20 ~ 30): (0.1 ~ 1.5).
In this step, preferably, a is 0.35, b be 0.25, c be 0.16, d be 0.25, x is 0.08.
Be appreciated that in this step and also can take ZrO
2, Yb
2o
3and Nd
2o
3each powder is in molar ratio for being preferably 35: 26: 13: 25: 1.
Step S13, the powder taken mixed obtain presoma in step S11.
In this step, powder is ground in corundum alms bowl body the presoma obtaining for 20 minutes ~ 60 minutes mixing, preferred grinding 40 minutes.
Step S15, by presoma calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C, be cooled to 100 DEG C ~ 300 DEG C afterwards, then be incubated 0.5 hour ~ 3 hours and obtain dysprosium doped titanium barium glass up-conversion luminescent material.
Preferably, presoma calcination 3 hours at 950 DEG C.
Preferably, at 800 DEG C ~ 1000 DEG C, calcination is cooled to 200 DEG C after 0.5 hour ~ 5 hours, then is incubated 2 hours.
Preferably, presoma puts into retort furnace calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C, be cooled to 100 DEG C ~ 300 DEG C afterwards, after being incubated 0.5 hour ~ 3 hours again, furnace cooling obtains bulk material to room temperature, then bulk material pulverizing is obtained dysprosium doped titanium barium glass up-conversion luminescent material.
The preparation method of above-mentioned dysprosium doped titanium barium glass 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 the dysprosium doped titanium barium glass up-conversion luminescent material of preparation, the excitation wavelength of dysprosium doped titanium barium glass up-conversion luminescent material is 796nm, in 482nm wavelength zone by Dy
3+ion
4f
9/2 → 6f
15/2transition radiation form glow peak, achieve that to inspire blue light shortwave by the infrared long-wave radiation to green glow luminous.
Refer to Fig. 1, the Organic Light Emitting Diode 100 of one embodiment, this Organic Light Emitting Diode 100 comprises the substrate 1, negative electrode 2, organic luminous layer 3, the transparent anode 4 that stack gradually and is mixed with the transparent encapsulated layer 5 of up-conversion phosphor 6, little dot fluorescent powder 6 material in transparent encapsulated layer 5 is dysprosium doped titanium barium glass up-conversion luminescent material, and its chemical formula is aTiO
2-bBaO-cB
2o
3-dSiO
2: xDy
3+, wherein, a is 0.3 ~ 0.4, b be 0.2 ~ 0.3, c be 0.1 ~ 0.2, d be 0.2 ~ 0.3, x is 0.001 ~ 0.01.
Organic luminous layer 3 in this device sends red-green glow, and part red-green glow excites in transparent encapsulated layer 5 and is dispersed with neodymium ytterbium codoped zirconium white up-conversion luminescent material 6 and sends blue light, and last redgreenblue just blendes together white light.
Be specific embodiment below.
Embodiment 1
Select purity be 99.99% powder, TiO
2, BaCO
3, H
3bO
3, SiO
2and Dy
2o
3powder, its mol ratio is 35: 26: 13: 25: 1, in corundum mortar, grinding makes its Homogeneous phase mixing in 40 minutes, then calcination 3 hours at 950 DEG C, be then cooled to 200 DEG C to be incubated 2 hours, then furnace cooling takes out to room temperature, obtain block materials, can obtain chemical general formula after pulverizing is 0.35TiO
2-0.26BaO-0.13B
2o
3-0.25SiO
2: 0.01Dy
3+up-conversion phosphor.
Refer to Fig. 2, the excitation wavelength of the dysprosium doped titanium barium glass up-conversion luminescent material that the present embodiment obtains is 796nm, when material is subject to the radiation of long wavelength (as 796nm) time, and Dy
3+the energy of this illumination of ionic absorption, now Dy
3+ion has just been in
4f
9/2excited state, then to
6f
15/2transition, just sends the blue light of 482nm, can as blue light emitting material.
Embodiment 2
Select purity be 99.99% powder, TiO
2, BaCO
3, H
3bO
3, SiO
2and Dy
2o
3powder, its mol ratio is 39.9: 30: 10: 20: 0.1, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, then calcination 0.5 hour at 1100 DEG C, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is 0.39.9TiO
2-0.30BaO-0.10B
2o
3-0.20SiO
2: 0.001Dy
3+up-conversion phosphor.
Embodiment 3
Select purity be 99.99% powder, TiO
2, BaCO
3, H
3bO
3, SiO
2and Dy
2o
3powder, its mol ratio is 30.5: 22: 16: 30: 1.5, in corundum mortar, grinding makes its Homogeneous phase mixing in 60 minutes, then calcination 5 hours at 800 DEG C, then 300 DEG C are cooled to be incubated 0.5 hour, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is 0.305TiO
2-0.22BaO-0.16B
2o
3-0.30SiO
2: 0.015Dy
3+up-conversion phosphor.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not 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 dysprosium doped titanium barium glass up-conversion luminescent material, is characterized in that: its chemical formula is aTiO
2-bBaO-cB
2o
3-dSiO
2: xDy
3+, wherein, a is 0.3 ~ 0.4, b be 0.2 ~ 0.3, c be 0.1 ~ 0.2, d be 0.2 ~ 0.3, x is 0.001 ~ 0.01.
2. dysprosium doped titanium barium glass up-conversion luminescent material according to claim 1, is characterized in that, a is 0.35, b be 0.25, c be 0.16, d be 0.25, x is 0.08.
3. a preparation method for dysprosium doped titanium barium glass up-conversion luminescent material, is characterized in that, comprise the following steps:
Step one, according to TiO
2, BaCO
3, H
3bO
3, SiO
2and Dy
2o
3each powder is (32 ~ 40) in molar ratio: (22 ~ 30): (10 ~ 16): (20 ~ 30): (0.1 ~ 1.5);
Step 2, the powder taken mixed obtain presoma in step one;
Step 3, by the calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C of described presoma, be cooled to 100 DEG C ~ 300 DEG C afterwards, then be incubated 0.5 hour ~ 3 hours and obtain dysprosium doped titanium barium glass up-conversion luminescent material, wherein chemical formula is aTiO
2-bBaO-cB
2o
3-dSiO
2: xDy
3+, wherein, a is 0.3 ~ 0.4, b be 0.2 ~ 0.3, c be 0.1 ~ 0.2, d be 0.2 ~ 0.3, x is 0.001 ~ 0.01.
4. the preparation method of dysprosium doped titanium barium glass up-conversion luminescent material according to claim 3, is characterized in that, a is 0.35, b be 0.25, c be 0.16, d be 0.25, x is 0.08.
5. the preparation method of dysprosium doped titanium barium glass up-conversion luminescent material according to claim 3, is characterized in that, is ground 20 minutes ~ 60 minutes by powder in step 2 in corundum alms bowl body.
6. the preparation method of dysprosium doped titanium barium glass up-conversion luminescent material according to claim 3, is characterized in that, by the calcination 3 hours at 950 DEG C of described presoma in step 3.
7. the preparation method of dysprosium doped titanium barium glass up-conversion luminescent material according to claim 3, it is characterized in that, by the calcination 3 hours at 950 DEG C of described presoma in step 3, be cooled to 200 DEG C afterwards, then be incubated 2 hours and obtain dysprosium doped titanium barium glass up-conversion luminescent material.
8. the preparation method of dysprosium doped titanium barium glass up-conversion luminescent material according to claim 3, it is characterized in that, the calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C of presoma described in step 3, be cooled to 100 DEG C ~ 300 DEG C afterwards, after being incubated 0.5 hour ~ 3 hours again, furnace cooling obtains bulk material to room temperature, is pulverized by described bulk material and obtains target product.
9. the preparation method of dysprosium doped titanium barium glass up-conversion luminescent material according to claim 3, is characterized in that, in step 2, the powder ball milling taken is obtained the presoma mixed in step one.
10. an Organic Light Emitting Diode, this Organic Light Emitting Diode comprises the substrate, negative electrode, organic luminous layer, the transparent anode that stack gradually and is mixed with the transparent encapsulated layer of up-conversion phosphor, it is characterized in that, the material of described up-conversion phosphor is dysprosium doped titanium barium glass up-conversion luminescent material, and the chemical formula of this dysprosium doped titanium barium glass up-conversion luminescent material is aTiO
2-bBaO-cB
2o
3-dSiO
2: xDy
3+, wherein, a is 0.3 ~ 0.4, b be 0.2 ~ 0.3, c be 0.1 ~ 0.2, d be 0.2 ~ 0.3, x is 0.001 ~ 0.01.
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| CN101353578A (en) * | 2008-09-05 | 2009-01-28 | 浙江大学 | Upconversion luminescent material |
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| US7515332B2 (en) * | 2004-02-18 | 2009-04-07 | Nippon Sheet Glass Company, Limited | Glass composition that emits fluorescence in infrared wavelength region and method of amplifying signal light using the same |
| JP2009286681A (en) * | 2008-05-30 | 2009-12-10 | Ohara Inc | Luminescent glass and luminescent crystallized glass |
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| Title |
|---|
| Femtosecond laser induced space-selective precipitation of nonlinear optical crystals in rare-earth-doped glasses;Bin Zhu等;《OPTICS EXPRESS》;20070502;第15卷;6069-6074 * |
| 飞秒激光诱导Dy3+掺杂玻璃的上转换发光;张松敏等;《武汉理工大学学报》;20070531;第29卷;327-330 * |
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