CN103045245B - Praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, preparation method and application thereof - Google Patents
Praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, preparation method and application thereof Download PDFInfo
- Publication number
- CN103045245B CN103045245B CN201110314970.5A CN201110314970A CN103045245B CN 103045245 B CN103045245 B CN 103045245B CN 201110314970 A CN201110314970 A CN 201110314970A CN 103045245 B CN103045245 B CN 103045245B
- Authority
- CN
- China
- Prior art keywords
- titanium dioxide
- luminescent material
- conversion luminescent
- ytterbium codope
- codope titanium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
A kind of praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, its chemical formula is TiO
2: xPr
3+, yYb
3+, wherein 0.02≤x≤0.1,0.02≤y≤0.2.In the photoluminescence spectra of this praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, the excitation wavelength of praseodymium ytterbium codope titanium dioxide up-conversion luminescent material is 980nm, in 485nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation formed glow peak, can as blue light emitting material.The present invention also provides the preparation method of this praseodymium ytterbium codope titanium dioxide up-conversion luminescent material and uses the Organic Light Emitting Diode of this praseodymium ytterbium codope titanium dioxide up-conversion luminescent material.
Description
[technical field]
The present invention relates to a kind of praseodymium ytterbium codope titanium dioxide 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 praseodymium ytterbium codope titanium dioxide 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 praseodymium ytterbium codope titanium dioxide up-conversion luminescent material of blue light, preparation method by long-wave radiation and use the Organic Light Emitting Diode of this praseodymium ytterbium codope titanium dioxide up-conversion luminescent material.
A kind of praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, its chemical formula is TiO
2: xPr
3+, yYb
3+, wherein 0.02≤x≤0.1,0.02≤y≤0.2.
In a preferred embodiment, x is 0.06, y is 0.1.
A preparation method for praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, comprises the following steps: step one, according to TiO
2: xPr
3+, yYb
3+the stoichiometric ratio of each element takes TiO
2, Pr
2o
3and Yb
2o
3powder, wherein 0.02≤x≤0.1,0.02≤y≤0.2; 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 ~ 500 DEG C afterwards, then be incubated 0.5 hour ~ 3 hours and obtain praseodymium ytterbium codope titanium dioxide up-conversion luminescent material.
In a preferred embodiment, x is 0.06, y is 0.1.
In a preferred embodiment, in step 2, powder is ground 20 minutes ~ 60 minutes in corundum alms bowl body.
In a preferred embodiment, step 3 kind is by the calcination 3 hours at 950 DEG C of described presoma.
In a preferred embodiment, in step 3 by described presoma calcination at 950 DEG C 3 hours, be cooled to 250 DEG C afterwards, then be incubated 2 hours and obtain praseodymium ytterbium codope titanium dioxide 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 ~ 500 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 substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer that stack gradually, be dispersed with praseodymium ytterbium codope titanium dioxide up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of described praseodymium ytterbium codope titanium dioxide up-conversion luminescent material is TiO
2: xPr
3+, yYb
3+, wherein 0.02≤x≤0.1,0.02≤y≤0.2.
The preparation method of above-mentioned praseodymium ytterbium codope titanium dioxide 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 praseodymium ytterbium codope titanium dioxide up-conversion luminescent material of preparation, the excitation wavelength of praseodymium ytterbium codope titanium dioxide up-conversion luminescent material is 980nm, in 485nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation formed glow peak, can as blue light emitting material.
[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 praseodymium ytterbium codope titanium dioxide up-conversion luminescent material prepared by embodiment 1.
Fig. 3 is the XRD spectra of praseodymium ytterbium codope titanium dioxide up-conversion luminescent material prepared by embodiment 1.
[embodiment]
Below in conjunction with the drawings and specific embodiments, praseodymium ytterbium codope titanium dioxide up-conversion luminescent material and preparation method thereof is illustrated further.
The praseodymium ytterbium codope titanium dioxide up-conversion luminescent material of one embodiment, its chemical formula is TiO
2: xPr
3+, yYb
3+, wherein 0.02≤x≤0.1,0.02≤y≤0.2.
Preferably, x is 0.06, y is 0.1.
In the photoluminescence spectra of this praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, the excitation wavelength of praseodymium ytterbium codope titanium dioxide up-conversion luminescent material is 980nm, when material is subject to the radiation of long wavelength (as 980nm) time, and Yb
3+the energy of this illumination of ionic absorption, then passes to Pr
3+ion.Now Pr
3+ion has just been in
3p
0excited state, then to
3h
4transition, just sends the blue light of 485nm,
The preparation method of above-mentioned praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, comprises the following steps:
Step S11, according to TiO
2: xPr
3+, yYb
3+the stoichiometric ratio of each element takes TiO
2, Pr
2o
3and Yb
2o
3powder, wherein 0.02≤x≤0.1,0.02≤y≤0.2.
In this step, preferably, x is 0.06, y is 0.1.
Be appreciated that in this step and also can take TiO
2, Pr
2o
3and Yb
2o
3powder also mixes, wherein TiO
2, Pr
2o
3and Yb
2o
3mass ratio be 0.68 ~ 0.784: 0.033 ~ 0.165: 0.039 ~ 0.394, be preferably 0.736: 0.099: 0.197.
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 ~ 500 DEG C afterwards, then be incubated 0.5 hour ~ 3 hours and obtain praseodymium ytterbium codope titanium dioxide 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 250 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 ~ 500 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 praseodymium ytterbium codope titanium dioxide up-conversion luminescent material.
The preparation method of above-mentioned praseodymium ytterbium codope titanium dioxide 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 praseodymium ytterbium codope titanium dioxide up-conversion luminescent material of preparation, the excitation wavelength of praseodymium ytterbium codope titanium dioxide up-conversion luminescent material is 980nm, in 485nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation formed glow peak, can as blue light emitting material.
Refer to Fig. 1, this Organic Light Emitting Diode 100 of the Organic Light Emitting Diode 100 of an embodiment comprises the substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the transparent encapsulated layer 5 that stack gradually.Be dispersed with praseodymium ytterbium codope titanium dioxide up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of praseodymium ytterbium codope titanium dioxide up-conversion luminescent material is TiO
2: xPr
3+, yYb
3+, wherein 0.02≤x≤0.1,0.02≤y≤0.2.
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, Pr
2o
3and Yb
2o
3powder, its mass ratio is 0.736g: 0.099g: 0.197g.In corundum mortar, grinding makes its Homogeneous phase mixing in 40 minutes, then calcination 3 hours at 950 DEG C.Then be cooled to 250 DEG C to be incubated 2 hours, then naturally cool to room temperature taking-up block product, and pulverized, obtaining chemical general formula is TiO
2: 0.06Pr
3+, 0.1Yb
3+up-conversion phosphor.
Refer to Fig. 2, Figure 2 shows that (chemical general formula is TiO for the sample of praseodymium ytterbium codope titanium dioxide up-conversion luminescent material and the ytterbium that undopes obtained
2: 0.06Pr
3+) photoluminescence spectra figure.As seen from Figure 2, the excitation wavelength of the praseodymium ytterbium codope titanium dioxide up-conversion luminescent material that the present embodiment obtains is 980nm, in 485nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation formed glow peak, this praseodymium ytterbium codope titanium dioxide up-conversion luminescent material can be used as blue light emitting material.
Refer to Fig. 3, in Fig. 3, curve is the XRD curve of praseodymium ytterbium codope titanium dioxide up-conversion luminescent material prepared by enforcement 1, test comparison standard P DF card.Contrast PDF card, diffraction peak is depicted as the crystal orientation of titanium dioxide, does not occur illustrating that two kinds of elements are the lattices entering titanium dioxide in the peak that praseodymium ytterbium element is relevant.
Embodiment 2
Select purity be 99.99% powder, TiO
2, Pr
2o
3and Yb
2o
3powder, its mass ratio is 0.784g: 0.033g: 0.039g.In corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, then calcination 5 hours at 800 DEG C.Then be cooled to 100 DEG C to be incubated 3 hours, then naturally cool to room temperature taking-up block product, and pulverized, obtain TiO
2: 0.02Pr
3+, 0.02Yb
3+up-conversion phosphor.
Embodiment 3
Select purity be 99.99% powder, TiO
2, Pr
2o
3and Yb
2o
3powder, its mass ratio is 0.68g: 0.165g: 0.394g.。In corundum mortar, grinding makes its Homogeneous phase mixing in 60 minutes, then calcination 0.5 hour at 1000 DEG C.Then be cooled to 500 DEG C to be incubated 0.5 hour, then naturally cool to room temperature taking-up block product, and pulverized, obtain TiO
2: 0.1Pr
3+, 0.2Yb
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 (1)
1. a preparation method for praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, is characterized in that, comprise the following steps:
Step one, according to TiO
2: xPr
3+, yYb
3+the stoichiometric ratio of each element takes TiO
2, Pr
2o
3and Yb
2o
3powder, wherein x is 0.06, y is 0.1;
Step 2, the powder taken mixed obtain presoma in step one;
Step 3, by the calcination 3 hours at 950 DEG C of described presoma, be cooled to 250 DEG C afterwards, then after being incubated 2 hours, furnace cooling obtains bulk material to room temperature, described bulk material is pulverized and obtains praseodymium ytterbium codope titanium dioxide up-conversion luminescent material;
In step 2, powder is ground 20 minutes ~ 60 minutes in corundum alms bowl body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110314970.5A CN103045245B (en) | 2011-10-17 | 2011-10-17 | Praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110314970.5A CN103045245B (en) | 2011-10-17 | 2011-10-17 | Praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103045245A CN103045245A (en) | 2013-04-17 |
| CN103045245B true CN103045245B (en) | 2015-11-25 |
Family
ID=48058110
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110314970.5A Active CN103045245B (en) | 2011-10-17 | 2011-10-17 | Praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103045245B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108485663A (en) * | 2016-04-13 | 2018-09-04 | 大连民族大学 | Rare earth mixing with nano ball-type TiO2The application of upper transition compounds |
| CN105938875B (en) * | 2016-07-12 | 2018-08-14 | 深圳市华星光电技术有限公司 | WOLED device architectures and display device |
| CN109148709B (en) * | 2018-09-04 | 2020-09-22 | 合肥鑫晟光电科技有限公司 | Electroluminescent display panel and display device |
| CN113980679A (en) * | 2021-09-03 | 2022-01-28 | 昆明理工大学 | TiO 22Preparation and application of Yb, Er up-conversion luminescence anti-counterfeiting fluorescent powder |
| CN116064036A (en) * | 2023-01-16 | 2023-05-05 | 海南大学 | Up-conversion luminescent material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177611A (en) * | 2007-12-07 | 2008-05-14 | 哈尔滨工业大学 | High luminous intensity up-conversion fluorescence nano-crystal oxide and preparation method thereof |
| CN101787272A (en) * | 2009-01-23 | 2010-07-28 | E.I.内穆尔杜邦公司 | Nano fluorescent particles doping with rare-earth ions and relevant application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011088223A1 (en) * | 2010-01-13 | 2011-07-21 | The Penn State Research Foundation | Up-conversion luminescent coatings/materials for antimicrobial applications |
-
2011
- 2011-10-17 CN CN201110314970.5A patent/CN103045245B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177611A (en) * | 2007-12-07 | 2008-05-14 | 哈尔滨工业大学 | High luminous intensity up-conversion fluorescence nano-crystal oxide and preparation method thereof |
| CN101787272A (en) * | 2009-01-23 | 2010-07-28 | E.I.内穆尔杜邦公司 | Nano fluorescent particles doping with rare-earth ions and relevant application thereof |
Non-Patent Citations (3)
| Title |
|---|
| 980nm激发下稀土掺杂TiO2纳米晶体的上转换发光研究;于辉;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20071115(第5期);B014-42 * |
| The influence of Yb3+ doping on the upconversion luminescence of Pr3+ in aluminum oxide based powders prepared by combustion synthesis;G.S. Maciel等;《Optical Materials》;20090623;第31卷;1735–1740 * |
| 稀土掺杂TiO2纳米晶体的制备及其上转换发光特性研究;张振众等;《武汉理工大学硕士学位论》;20090915;1-57 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103045245A (en) | 2013-04-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103045245B (en) | Praseodymium ytterbium codope titanium dioxide up-conversion luminescent material, preparation method and application thereof | |
| CN102952543B (en) | Thulium-holmium co-doped zirconia upconversion phosphor and preparation method thereof | |
| CN103421491B (en) | Terbium ytterbium codoped C 12 A 7 base up-conversion luminescent material, preparation method and Organic Light Emitting Diode | |
| CN104099091A (en) | Neodymium-and-ytterbium-codoped alkaline earth fluoride glass up-conversion luminescent material, and preparation method and application thereof | |
| CN103045246B (en) | Neodymium-ytterbium-codoped zirconia up-conversion luminescent material as well as preparation method and application thereof | |
| CN103059858A (en) | Yttrium silicate upconversion luminous fluorescent powder, preparation method and application thereof | |
| CN103045240B (en) | Thulium doped strontium aluminate up-conversion luminescent material, preparation method and application thereof | |
| CN103045253A (en) | Thulium doped lithium lanthanum molybdate up-conversion luminescent material, preparation method and application thereof | |
| CN104650882A (en) | Terbium/ytterbium-codoped alkali gallium tungstate up-conversion luminescent material, preparation method and application thereof | |
| CN103045243B (en) | Praseodymium and ytterbium codope fluoborate glass up-conversion luminescent material and preparation method and application thereof | |
| CN103965896A (en) | Praseodymium holmium co-doped zirconium aluminium oxide glass upconversion luminescence material, and preparation method and application thereof | |
| CN103045237B (en) | Neodymium-ytterbium double-doped barium chloride up-conversion luminescent material as well as preparation method and application thereof | |
| CN103045252A (en) | Praseodymium and ytterbium codope gadolinium oxide up-conversion luminescent material and preparation method and application thereof | |
| CN103450896A (en) | Thulium-doped fluoroaluminate up-conversion fluorescent powder and preparation method thereof | |
| CN103059853B (en) | Titanate phosphors for up-conversion luminescence, and preparation method and application thereof | |
| CN103045244B (en) | Dysprosium doped barium titanium glass up-conversion luminescent material, preparation method and application thereof | |
| CN104745182A (en) | Neodymium-doped chlorogermanate up-conversion phosphor and preparation method thereof | |
| CN104650910A (en) | Praseodymium-doped cerium phosphate up-conversion luminescent material, and preparation method and application thereof | |
| CN103059867B (en) | Tellurate phosphors for up-conversion luminescence, and preparation method and application thereof | |
| CN103059866B (en) | Neodymium ytterbium doped halide upconversion luminous fluorescent powder, preparation method and application thereof | |
| CN103059851B (en) | Bismuthate upconversion luminous fluorescent powder, preparation method and application thereof | |
| CN104099090A (en) | Dysprosium-doped alkali fluosilicic acid glass up-conversion luminescent material, and preparation method and application thereof | |
| CN104178161A (en) | Samarium- ytterbium- co-doped rare earth gallate up-conversion luminescent materials, and preparing method and applications thereof | |
| CN103059844A (en) | Sulfide upconversion luminous fluorescent powder, preparation method and application thereof | |
| CN103965901A (en) | Praseodymium-ytterbium-codoped lead-cadmium fluoride glass up-conversion luminescent material and its preparation method and use |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |