CN104099095A - Neodymium-and-ytterbium-codoped stannic fluoride glass up-conversion luminescent material, and preparation method and application thereof - Google Patents
Neodymium-and-ytterbium-codoped stannic fluoride glass up-conversion luminescent material, and preparation method and application thereof Download PDFInfo
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- CN104099095A CN104099095A CN201310121307.2A CN201310121307A CN104099095A CN 104099095 A CN104099095 A CN 104099095A CN 201310121307 A CN201310121307 A CN 201310121307A CN 104099095 A CN104099095 A CN 104099095A
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Abstract
The invention provides a neodymium-and-ytterbium-codoped stannic fluoride glass up-conversion luminescent material. The chemical formula of the luminescent material is SnF4: xYb3+,yNd3+, wherein x is in a range of 0.005 to 0.05, and y is in a range of 0.002 to 0.03. In the photoluminescence spectrum of the neodymium-and-ytterbium-codoped stannic fluoride glass up-conversion luminescent material, the excitation wavelength of the neodymium-and-ytterbium-codoped stannic fluoride glass up-conversion luminescent material is 586 nm, and in the wavelength zone of 469 nm, a luminescence peak is formed by transition radiation of Nd3+ ions from 2P3/2 to 4I15/2; and the material can be used as a blue-light luminescent material. The invention further provides a preparation method for the neodymium-and-ytterbium-codoped stannic fluoride glass up-conversion luminescent material and an organic light-emitting diode using the neodymium-and-ytterbium-codoped stannic fluoride glass up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass, 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 be short, flexible, and obtained the utmost point, apply widely.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, can be by infrared, the long-wave radiations such as red-green glow inspire the neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass of blue emission, have not yet to see report.
Summary of the invention
Based on this, being necessary to provide a kind of can be inspired neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass, the preparation method of blue light and be used the Organic Light Emitting Diode of this neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass by long-wave radiation.
A neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass, its chemical formula is SnF
4: xYb
3+, yNd
3+, wherein, x is that 0.005～0.05, y is 0.002～0.03.
Described x is that 0.03, y is 0.03.
A preparation method for neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass, comprises the following steps
Step 1, according to SnF
4: xYb
3+, yNd
3+the stoichiometric ratio of each element takes SnF
4, YbF
3and NdF
3powder, wherein, x is that 0.005～0.05, y is 0.002～0.03;
Step 2, the powder taking in described step 1 is mixed and obtains presoma;
Step 3, by the calcination 0.5 hour～5 hours at 800 ℃～1100 ℃ of the presoma in described step 2;
Step 4, the precursor after processing in described step 3 is cooled to 100 ℃～300 ℃, then is incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is SnF
4: xYb
3+, yNd
3+neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass.
Described SnF
4, YbF
3and NdF
3each component mol ratio of powder is (92～99.3): (0.5～5): (0.2～3).
Described SnF
4, YbF
3and NdF
3each component mol ratio of powder is 96:3:1.
Described in step 2, mixing is described powder to be ground in corundum alms bowl 20 minutes～60 minutes.
In step 3 by the calcination 3 hours at 950 ℃ of described presoma.
Cooling temperature in step 4 is 250 ℃, and soaking time is 2 hours.
A kind of Organic Light Emitting Diode, comprise the substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer that stack gradually, it is characterized in that, in described transparent encapsulated layer, be dispersed with neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass, the chemical formula of described neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass is SnF
4: xYb
3+, yNd
3+, wherein, x is that 0.005～0.05, y is 0.002～0.03.
X is that 0.03, y is 0.03.
The preparation method of above-mentioned neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass is comparatively simple, and cost is lower, produces comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass of preparation, the excitation wavelength of neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass is 586nm, in 469nm wavelength zone by Nd
3+ion
2p
3/2→
4i
15/2transition radiation form glow peak, can be used 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 the neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass of embodiment 1 preparation.
Fig. 3 is the XRD spectra of the neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass of embodiment 1 preparation.
Fig. 4 forms the spectrogram of the Organic Light Emitting Diode emitting white light doped with neodymium ytterbium codoped Tin tetrafluoride. changing luminous material material on glass in the transparent encapsulated layer of embodiment 1 preparation.
Embodiment
Below in conjunction with the drawings and specific embodiments, neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass and preparation method thereof is further illustrated.
The neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass of one embodiment, its chemical formula is SnF
4: xYb
3+, yNd
3+, wherein, x is that 0.005～0.05, y is 0.002～0.03.
Preferably, x is that 0.03, y is 0.03.
In the photoluminescence spectra of this neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass, the excitation wavelength of neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass is 586nm, when material is subject to long wavelength's (as 586nm) radiation, and Nd
3+ion just in
2p
3/2excited state, then to
4i
15/2transition, just sends the blue light of 469nm, can be used as blue light emitting material.
The preparation method of above-mentioned neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass, comprises the following steps:
Step S11, according to SnF
4: xYb
3+, yNd
3+the stoichiometric ratio of each element takes SnF
4, YbF
3and NdF
3powder, wherein, x is that 0.005～0.05, y is 0.002～0.03.
In this step, described SnF
4, YbF
3and NdF
3each component mol ratio of powder is (92～99.3): (0.5～5): (0.2～3).
In this step, preferred, SnF
4, YbF
3and NdF
3each component mol ratio of powder is 96:3:1.
Step S13, the powder taking in step S11 is mixed and obtains presoma.
In this step, powder is ground in corundum alms bowl to the 20 minutes～presoma that obtains mixing for 60 minutes, preferably grind 40 minutes.
Step S15, by presoma calcination 0.5 hour～5 hours at 800 ℃～1100 ℃,
Preferably, presoma calcination 3 hours at 950 ℃.
After step S17, the precursor after will be in step S15 processing, be cooled to 100 ℃～500 ℃, then be incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is SnF
4: xYb
3+, yNd
3+neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass, wherein, x is that 0.005～0.05, y is 0.002～0.03.
Preferably, the precursor after processing in step S15 is cooled to 200 ℃, then is incubated 2 hours.
The preparation method of above-mentioned neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass is comparatively simple, and cost is lower, produces comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass of preparation, the excitation wavelength of neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass is 586nm, in 469nm wavelength zone by Nd
3+ion
2p
3/2→
4i
15/2transition radiation form glow peak, can be used as blue light emitting material.
Refer to Fig. 1, the Organic Light Emitting Diode 100 of an embodiment, this Organic Light Emitting Diode 100 comprises substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the transparent encapsulated layer 5 stacking gradually.In transparent encapsulated layer 5, be dispersed with neodymium ytterbium codoped Tin tetrafluoride. changing luminous material 6 on glass, the chemical formula of neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass is SnF
4: xYb
3+, yNd
3+, wherein, x is 0.005～0.05, y is 0.002～0.03, organic luminous layer 3 in this device sends red-green glow, and part red-green glow excites and in transparent encapsulated layer 5, is dispersed with neodymium ytterbium codoped Tin tetrafluoride. changing luminous material 6 on glass and sends blue light, and last redgreenblue just blendes together white light.
Be specific embodiment below.
Embodiment 1
Selecting purity is 99.99% powder, by SnF
4, YbF
3and NdF
3each component of powder is 0.96mmol by mole number, 0.03mmol, 0.01mmol grinds and it was evenly mixed in 40 minutes in corundum mortar, then calcination 3 hours at 950 ℃ in retort furnace, then be cooled to 250 ℃ of insulations 2 hours, furnace cooling takes out to room temperature again, obtains block materials, and after pulverizing, can obtain chemical general formula is SnF
4: 0.03Yb
3+, 0.01Nd
3+up-conversion phosphor.
Process prepared by Organic Light Emitting Diode
The substrate 1 stacking gradually uses soda-lime glass, negative electrode 2 to use metal A g layer, organic luminous layer 3 to use Ir (piq) 2 (acac) Chinese name to close iridium (III), transparent anode 4 use tin indium oxide ITO two (1-phenyl-isoquinoline 99.9) (methyl ethyl diketones), and transparent encapsulated layer 5 tetrafluoroethylene.In transparent encapsulated layer 5, be dispersed with neodymium ytterbium codoped Tin tetrafluoride. changing luminous material 6 on glass, the chemical formula of neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass is SnF
4: 0.03Yb
3+, 0.01Nd
3+.
Refer to Fig. 2, Figure 2 shows that the photoluminescence spectra figure of the neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass obtaining.As seen from Figure 2, the excitation wavelength of the neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass that curve 1 the present embodiment obtains is 586nm, in 469nm wavelength zone by Nd
3+ion
2p
3/2→
4i
15/2transition radiation form glow peak, this neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass can be used as blue light emitting material, curve 2 is the Tin tetrafluoride. changing luminous material on glass of the ytterbium element that do not adulterate, and the sample that has increased as seen from the figure ytterbium element codoped has higher luminous efficiency.
Refer to Fig. 3, in Fig. 3, curve is for implementing the XRD curve of the neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass of 1 preparation, test comparison standard P DF card.Contrast PDF card, can find out that all diffraction peaks are all the crystallization phasess of corresponding Tin tetrafluoride., and does not have doped element and other dephasign to occur, illustrates that the product that this preparation method obtains has good crystalline quality.
Refer to Fig. 4, Fig. 4 curve 1 is for form the spectrogram of the Organic Light Emitting Diode emitting white light in transparent encapsulated layer doped with neodymium ytterbium codoped Tin tetrafluoride. changing luminous material material on glass, and curve 2 is not doped with the contrast of neodymium ytterbium codoped Tin tetrafluoride. changing luminous material material on glass in transparent encapsulated layer.In figure, can find out, fluorescent material can inspire the blue light of shortwave by the red light of long wave, blendes together white light.
Embodiment 2
Selecting purity is 99.99% powder, by SnF
4, YbF
3and NdF
3each component of powder is 0.965mmol by mole number, 0.005mmol, 0.03mmol grinds and it was evenly mixed in 20 minutes in corundum mortar, then calcination 3 hours at 800 ℃ in retort furnace, then be cooled to 250 ℃ of insulations 2 hours, furnace cooling takes out to room temperature again, obtains block materials, and after pulverizing, can obtain chemical general formula is SnF
4: 0.005Yb
3+, 0.03Nd
3+up-conversion phosphor.
Embodiment 3
Selecting purity is 99.99% powder, by SnF
4, YbF
3and NdF
3each component of powder is 0.948mmol by mole number, 0.05mmol, 0.002mmol, in corundum mortar, grind and it was evenly mixed in 60 minutes, then calcination 3 hours at 1000 ℃ in retort furnace, be then cooled to 250 ℃ of insulations 2 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is SnF
4: 0.05Yb
3+, 0.002Nd
3+up-conversion phosphor.
Embodiment 4
Selecting purity is 99.99% powder, by SnF
4, YbF
3and NdF
3each component of powder is 0.98mmol by mole number, 0.01mmol, 0.01mmol, in corundum mortar, grind and it was evenly mixed in 50 minutes, then calcination 3 hours at 900 ℃ in retort furnace, be then cooled to 250 ℃ of insulations 2 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is SnF
4: 0.01Yb
3+, 0.01Nd
3+up-conversion phosphor.
Embodiment 5
Selecting purity is 99.99% powder, by SnF
4, YbF
3and NdF
3each component of powder is 0.96mmol by mole number, 0.02mmol, 0.02mmol, in corundum mortar, grind and it was evenly mixed in 30 minutes, then calcination 3 hours at 980 ℃ in retort furnace, be then cooled to 250 ℃ of insulations 2 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is SnF
4: 0.02Yb
3+, 0.02Nd
3+up-conversion phosphor.
Embodiment 6
Selecting purity is 99.99% powder, by SnF
4, YbF
3and NdF
3each component of powder is 0.93mmol by mole number, 0.04mmol, 0.03mmol, in corundum mortar, grind and it was evenly mixed in 55 minutes, then calcination 3 hours at 850 ℃ in retort furnace, be then cooled to 250 ℃ of insulations 2 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is SnF
4: 0.04Yb
3+, 0.03Nd
3+up-conversion phosphor.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore 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 neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass, is characterized in that: its chemical general formula is SnF
4: xYb
3+, yNd
3+, wherein, x is that 0.005～0.05, y is 0.002～0.03.
2. neodymium ytterbium codoped Tin tetrafluoride. according to claim 1 changing luminous material on glass, is characterized in that, described x is that 0.03, y is 0.03.
3. a preparation method for neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass, is characterized in that, comprises the following steps:
Step 1, according to SnF
4: xYb
3+, yNd
3+the stoichiometric ratio of each element takes SnF
4, YbF
3and NdF
3powder, wherein, x is that 0.005～0.05, y is 0.002～0.03;
Step 2, the powder taking in described step 1 is mixed and obtains presoma;
Step 3, by the calcination 0.5 hour～5 hours at 800 ℃～1000 ℃ of described presoma;
Step 4, the precursor after processing in described step 3 is cooled to 100 ℃～300 ℃, then is incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is SnF
4: xYb
3+, yNd
3+neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass.
4. the preparation method of neodymium ytterbium codoped Tin tetrafluoride. according to claim 3 changing luminous material on glass, is characterized in that described SnF
4, YbF
3and NdF
3each component mol ratio of powder is (92～99.3): (0.5～5): (0.2～3).
5. the preparation method of neodymium ytterbium codoped Tin tetrafluoride. according to claim 3 changing luminous material on glass, is characterized in that described SnF
4, YbF
3and NdF
3each component mol ratio of powder is 96:3:1.
6. the preparation method of neodymium ytterbium codoped Tin tetrafluoride. according to claim 3 changing luminous material on glass, is characterized in that, described in step 2, mixing is described powder to be ground in corundum alms bowl 20 minutes～60 minutes.
7. the preparation method of neodymium ytterbium codoped Tin tetrafluoride. according to claim 3 changing luminous material on glass, is characterized in that, in step 3 by the calcination 3 hours at 950 ℃ of described presoma.
8. the preparation method of neodymium ytterbium codoped Tin tetrafluoride. according to claim 3 changing luminous material on glass, is characterized in that, the cooling temperature in step 4 is 250 ℃, and soaking time is 2 hours.
9. an Organic Light Emitting Diode, this Organic Light Emitting Diode comprises substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer stacking gradually, it is characterized in that, in described transparent encapsulated layer, be dispersed with neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass, the chemical formula of described neodymium ytterbium codoped Tin tetrafluoride. changing luminous material on glass is SnF
4: xYb
3+, yNd
3+, wherein, x is that 0.005～0.05, y is 0.002～0.03.
10. Organic Light Emitting Diode according to claim 9, is characterized in that, described x is that 0.03, y is 0.03.
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|---|---|---|---|
| CN201310121307.2A CN104099095A (en) | 2013-04-09 | 2013-04-09 | Neodymium-and-ytterbium-codoped stannic fluoride glass up-conversion luminescent material, and preparation method and application thereof |
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|---|---|---|---|
| CN201310121307.2A CN104099095A (en) | 2013-04-09 | 2013-04-09 | Neodymium-and-ytterbium-codoped stannic fluoride glass up-conversion luminescent material, and preparation method and application thereof |
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|---|---|
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ID=51667646
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|---|---|---|---|
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587141A (en) * | 2004-09-21 | 2005-03-02 | 同济大学 | Organic blended lead-tin-fluorine-phosphate flash glass and its preparing method |
| EP1666562A2 (en) * | 2004-11-11 | 2006-06-07 | Samsung Electronics Co., Ltd. | Interfused nanocrystals and method of preparing the same |
-
2013
- 2013-04-09 CN CN201310121307.2A patent/CN104099095A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587141A (en) * | 2004-09-21 | 2005-03-02 | 同济大学 | Organic blended lead-tin-fluorine-phosphate flash glass and its preparing method |
| EP1666562A2 (en) * | 2004-11-11 | 2006-06-07 | Samsung Electronics Co., Ltd. | Interfused nanocrystals and method of preparing the same |
Non-Patent Citations (1)
| Title |
|---|
| K. TOSHIMA，: ""Glycosyl fluorides in glycosidations"", 《CARBOHYDRATE RESEARCH》, vol. 327, 31 December 2000 (2000-12-31), pages 15 - 26, XP004215275, DOI: doi:10.1016/S0008-6215(99)00325-0 * |
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Application publication date: 20141015 |