CN104099091A - Neodymium-and-ytterbium-codoped alkaline earth fluoride glass up-conversion luminescent material, and preparation method and application thereof - Google Patents

Neodymium-and-ytterbium-codoped alkaline earth fluoride glass up-conversion luminescent material, and preparation method and application thereof Download PDF

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Publication number
CN104099091A
CN104099091A CN201310121321.2A CN201310121321A CN104099091A CN 104099091 A CN104099091 A CN 104099091A CN 201310121321 A CN201310121321 A CN 201310121321A CN 104099091 A CN104099091 A CN 104099091A
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alkaline earth
earth fluoride
glass
fluoride salt
luminous material
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周明杰
王平
陈吉星
黄辉
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

The invention provides a neodymium-and-ytterbium-codoped alkaline earth fluoride glass up-conversion luminescent material. The chemical formula of the luminescent material is MeF2: xYb3+,yNd3+, wherein x is in a range of 0.005 to 0.05, y is in a range of 0.002 to 0.03, and Me is one selected from the group consisting of magnesium, calcium, strontium and barium. In the photoluminescence spectrum of the neodymium-and-ytterbium-codoped alkaline earth fluoride glass up-conversion luminescent material, the excitation wavelength of the neodymium-and-ytterbium-codoped alkaline earth 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 alkaline earth fluoride glass up-conversion luminescent material and an organic light-emitting diode using the neodymium-and-ytterbium-codoped alkaline earth fluoride glass up-conversion luminescent material.

Description

Neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass, preparation method and application thereof
Technical field
The present invention relates to a kind of neodymium ytterbium codoped alkaline earth fluoride salt 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, apply widely and obtained the utmost point.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 alkaline earth fluoride salt 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 alkaline earth fluoride salt changing luminous material on glass, the preparation method of blue light and be used the Organic Light Emitting Diode of this neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass by long-wave radiation.
A kind of neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass, its chemical formula is MeF 2: xYb 3+, yNd 3+, wherein, x is that 0.005～0.05, y is that 0.002～0.03, Me is the one in magnesium, calcium, strontium and barium element.
Described x is that 0.03, y is 0.01.
A preparation method for neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass, comprises the following steps
Step 1, according to MeF 2: xYb 3+, yNd 3+the stoichiometric ratio of each element takes MeF 2, YbF 3and NdF 3powder, wherein, x is that 0.005～0.05, y is that 0.002～0.03, Me is the one in magnesium, calcium, strontium and barium element;
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 DEG C～1000 DEG C of the presoma in described step 2;
Step 4, precursor after treatment in described step 3 is cooled to 100 DEG C～500 DEG C, then is incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is MeF 2: xYb 3+, yNd 3+neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass.
Described MeF 2, YbF 3and NdF 3the each component mol ratio of powder is (92～99.3): (0.5～5): (0.2～3).
Described MeF 2, YbF 3and NdF 3the each 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 DEG C of described presoma.
Cooling temperature in step 4 is 250 DEG C, 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, in described transparent encapsulated layer, be dispersed with neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass, the chemical formula of described neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass is MeF 2: xYb 3+, yNd 3+, wherein, x is that 0.005～0.05, y is that 0.002～0.03, Me is the one in magnesium, calcium, strontium and barium element.
X is that 0.03, y is 0.01.
The preparation method of above-mentioned neodymium ytterbium codoped alkaline earth fluoride salt 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 alkaline earth fluoride salt changing luminous material on glass of preparation, the excitation wavelength of neodymium ytterbium codoped alkaline earth fluoride salt 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.
Brief description of the drawings
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 alkaline earth fluoride salt changing luminous material on glass prepared of embodiment 1.
Fig. 3 is the XRD spectrum of the neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass prepared of embodiment 1.
Fig. 4 is the spectrogram that forms the Organic Light Emitting Diode emitting white light in the transparent encapsulated layer prepared of embodiment 1 doped with neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material material on glass.
Embodiment
Below in conjunction with the drawings and specific embodiments, neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass and preparation method thereof is further illustrated.
The neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass of one embodiment, its chemical formula is MeF 2: xYb 3+, yNd 3+, wherein, x is that 0.005～0.05, y is that 0.002～0.03, Me is the one in magnesium, calcium, strontium and barium element.
Preferably, x is that 0.03, y is 0.01.
In the photoluminescence spectra of this neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass, the excitation wavelength of neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass is 586nm, in the time that 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 alkaline earth fluoride salt changing luminous material on glass, comprises the following steps:
Step S11, according to MeF 2: xYb 3+, yNd 3+the stoichiometric ratio of each element takes MeF 2, YbF 3and NdF 3powder, wherein, x is that 0.005～0.05, y is that 0.002～0.03, Me is the one in magnesium, calcium, strontium and barium element.
In this step, described MeF 2, YbF 3and NdF 3the each component mol ratio of powder is (92～99.3): (0.5～5): (0.2～3).
In this step, preferred, MeF 2, YbF 3and NdF 3the each 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 DEG C～1000 DEG C,
Preferably, presoma calcination 3 hours at 950 DEG C.
Step S17, will be cooled to 100 DEG C～500 DEG C after precursor after treatment in step S15, then be incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is MeF 2: xYb 3+, yNd 3+neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass, wherein, x is that 0.005～0.05, y is that 0.002～0.03, Me is the one in magnesium, calcium, strontium and barium element.
Preferably, precursor after treatment in step S15 is cooled to 500 DEG C, then is incubated 2 hours.
The preparation method of above-mentioned neodymium ytterbium codoped alkaline earth fluoride salt 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 alkaline earth fluoride salt changing luminous material on glass of preparation, the excitation wavelength of neodymium ytterbium codoped alkaline earth fluoride salt 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 the substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the transparent encapsulated layer 5 that stack gradually.In transparent encapsulated layer 5, be dispersed with neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material 6 on glass, the chemical formula of neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass is MeF 2: xYb 3+, yNd 3+wherein, x is 0.005～0.05, y is 0.002～0.03, Me is the one in magnesium, calcium, strontium and barium element, 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 alkaline earth fluoride salt 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 MgF 2, YbF 3and NdF 3the each 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 DEG C in retort furnace, then be cooled to 250 DEG C of insulations 2 hours, furnace cooling takes out to room temperature again, obtains block materials, and after pulverizing, can obtain chemical general formula is MgF 3: 0.03Yb 3+, 0.01Nd 3+up-conversion phosphor.
Process prepared by Organic Light Emitting Diode
The substrate 1 stacking gradually use soda-lime glass, negative electrode 2 use metal A g layer, organic luminous layer 3 use Ir (piq) 2 (acac) Chinese name two (1-phenyl-isoquinoline 99.9) (methyl ethyl diketones) close iridium (III), transparent anode 4 uses tin indium oxide ITO, and transparent encapsulated layer 5 tetrafluoroethylene.In transparent encapsulated layer 5, be dispersed with neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material 6 on glass, the chemical formula of neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass is MgF 3: 0.03Yb 3+, 0.01Nd 3+.
Refer to Fig. 2, Figure 2 shows that the photoluminescence spectra figure of the neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass obtaining.As seen from Figure 2, the excitation wavelength of the neodymium ytterbium codoped alkaline earth fluoride salt 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 alkaline earth fluoride salt changing luminous material on glass can be used as blue light emitting material, curve 2 is the rubidium doping alkaline earth fluoride salt changing luminous materials on glass of ytterbium element of not adulterating, and can find out and increase Yb 3+the codoped of element, sample has had better luminous efficiency.
Refer to Fig. 3, in Fig. 3, curve is the neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material XRD spectrum on glass figure that implements 1 preparation, can find out that the each element rule of light-emitting film prepared by the present embodiment arranges and formed the stable crystalline structure taking alkaline earth fluoride salt as matrix, there is not the crystallization phases separating, further illustrate doped element Uniform Doped and in the crystal of matrix, formed stable crystal.
Refer to Fig. 4, Fig. 4 curve 1 is for forming the spectrogram of the Organic Light Emitting Diode emitting white light doped with neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material material on glass in transparent encapsulated layer, curve 2 is the not contrast doped with neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material material on glass in transparent encapsulated layer.In figure, can find out, neodymium ytterbium codoped alkaline earth fluoride salt up-conversion luminescent material can, by the red light of long wave, inspire the blue light of shortwave, after blue light mixes with ruddiness, forms white light.
Embodiment 2
Selecting purity is 99.99% powder, by MgF 2, YbF 3and NdF 3the each 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 DEG C in retort furnace, then be cooled to 100 DEG C of insulations 3 hours, furnace cooling takes out to room temperature again, obtains block materials, and after pulverizing, can obtain chemical general formula is MgF 3: 0.005Yb 3+, 0.03Nd 3+up-conversion phosphor.
Embodiment 3
Selecting purity is 99.99% powder, by MgF 2, YbF 3and NdF 3the each 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 DEG C in retort furnace, be then cooled to 250 DEG C of insulations 2 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is MgF 2: 0.05Yb 3+, 0.002Nd 3+up-conversion phosphor.
Embodiment 4
Selecting purity is 99.99% powder, by CaF 2, YbF 3and NdF 3the each component of powder is 0.96mmol by mole number, 0.03mmol, 0.01mmol, 0.05mmol grinds and it was evenly mixed in 40 minutes in corundum mortar, then calcination 3 hours at 950 DEG C in retort furnace, be then cooled to 250 DEG C of insulations 2 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is CaF 3: 0.03Yb 3+, 0.01Nd 3+up-conversion phosphor.
Embodiment 5
Selecting purity is 99.99% powder, by CaF 2, YbF 3and NdF 3the each component of powder is 0.965mmol by mole number, 0.005mmol, 0.03mmol, in corundum mortar, grind and it was evenly mixed in 20 minutes, then calcination 3 hours at 800 DEG C in retort furnace, be then cooled to 250 DEG C of insulations 2 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is CaF 3: 0.005Yb 3+, 0.03Nd 3+up-conversion phosphor.
Embodiment 6
Selecting purity is 99.99% powder, by CaF 2, YbF 3and NdF 3the each 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 0.5 hour at 1000 DEG C in retort furnace, be then cooled to 500 DEG C of insulations 0.5 hour, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is CaF 2: 0.05Yb 3+, 0.002Nd 3+up-conversion phosphor.
Embodiment 7
Selecting purity is 99.99% powder, by SrF 2, YbF 3and NdF 3the each component of powder is 0.96mmol by mole number, 0.03mmol, 0.01mmol, in corundum mortar, grind and it was evenly mixed in 40 minutes, then calcination 3 hours at 950 DEG C in retort furnace, be then cooled to 250 DEG C of insulations 2 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is SrF 3: 0.03Yb 3+, 0.01Nd 3+up-conversion phosphor.
Embodiment 8
Selecting purity is 99.99% powder, by SrF 2, YbF 3and NdF 3the each component of powder is 0.965mmol by mole number, 0.005mmol, 0.03mmol, in corundum mortar, grind and it was evenly mixed in 20 minutes, then calcination 3 hours at 800 DEG C in retort furnace, be then cooled to 250 DEG C of insulations 2 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is SrF 3: 0.005Yb 3+, 0.03Nd 3+up-conversion phosphor.
Embodiment 9
Selecting purity is 99.99% powder, by SrF 2, YbF 3and NdF 3the each 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 DEG C in retort furnace, be then cooled to 250 DEG C of insulations 2 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is SrF 2: 0.05Yb 3+, 0.002Nd 3+up-conversion phosphor.
Embodiment 10
Selecting purity is 99.99% powder, by BaF 2, YbF 3and NdF 3the each component of powder is 0.96mmol by mole number, 0.03mmol, 0.01mmol, in corundum mortar, grind and it was evenly mixed in 40 minutes, then calcination 3 hours at 950 DEG C in retort furnace, be then cooled to 250 DEG C of insulations 2 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is BaF 3: 0.03Yb 3+, 0.01Nd 3+up-conversion phosphor.
Embodiment 11
Selecting purity is 99.99% powder, by BaF 2, YbF 3and NdF 3the each component of powder is 0.965mmol by mole number, 0.005mmol, 0.03mmol, in corundum mortar, grind and it was evenly mixed in 20 minutes, then calcination 3 hours at 800 DEG C in retort furnace, be then cooled to 250 DEG C of insulations 2 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is BaF 3: 0.005Yb 3+, 0.03Nd 3+up-conversion phosphor.
Embodiment 12
Selecting purity is 99.99% powder, by BaF 2, YbF 3and NdF 3the each 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 DEG C in retort furnace, be then cooled to 250 DEG C of insulations 2 hours, then furnace cooling takes out to room temperature, obtain block materials, after pulverizing, can obtain chemical general formula is BaF 2: 0.05Yb 3+, 0.002Nd 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 alkaline earth fluoride salt changing luminous material on glass, is characterized in that: its chemical general formula is MeF 2: xYb 3+, yNd 3+, wherein, x is that 0.005～0.05, y is that 0.002～0.03, Me is the one in magnesium, calcium, strontium and barium element.
2. neodymium ytterbium codoped alkaline earth fluoride salt according to claim 1 changing luminous material on glass, is characterized in that, described x is that 0.03, y is 0.01.
3. a preparation method for neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass, is characterized in that, comprises the following steps:
Step 1, according to MeF 2: xYb 3+, yNd 3+the stoichiometric ratio of each element takes MeF 2, YbF 3and NdF 3powder, wherein, x is that 0.005～0.05, y is that 0.002～0.03, Me is the one in magnesium, calcium, strontium and barium element;
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 DEG C～1000 DEG C of described presoma;
Step 4, precursor after treatment in described step 3 is cooled to 100 DEG C～500 DEG C, then is incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is MeF 2: xYb 3+, yNd 3+neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass.
4. the preparation method of neodymium ytterbium codoped alkaline earth fluoride salt according to claim 3 changing luminous material on glass, is characterized in that described MeF 2, YbF 3and NdF 3the each component mol ratio of powder is (92～99.3): (0.5～5): (0.2～3).
5. the preparation method of neodymium ytterbium codoped alkaline earth fluoride salt according to claim 3 changing luminous material on glass, is characterized in that described MeF 2, YbF 3and NdF 3the each component mol ratio of powder is 96:3:1.
6. the preparation method of neodymium ytterbium codoped alkaline earth fluoride salt 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 alkaline earth fluoride salt according to claim 3 changing luminous material on glass, is characterized in that, in step 3 by the calcination 3 hours at 950 DEG C of described presoma.
8. the preparation method of neodymium ytterbium codoped alkaline earth fluoride salt according to claim 3 changing luminous material on glass, is characterized in that, the cooling temperature in step 4 is 250 DEG C, and soaking time is 2 hours.
9. an 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, it is characterized in that, in described transparent encapsulated layer, be dispersed with neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass, the chemical formula of described neodymium ytterbium codoped alkaline earth fluoride salt changing luminous material on glass is MeF 2: xYb 3+, yNd 3+, wherein, x is that 0.005～0.05, y is that 0.002～0.03, Me is the one in magnesium, calcium, strontium and barium element.
10. Organic Light Emitting Diode according to claim 9, is characterized in that, described x is that 0.03, y is 0.01.
CN201310121321.2A 2013-04-09 2013-04-09 Neodymium-and-ytterbium-codoped alkaline earth fluoride glass up-conversion luminescent material, and preparation method and application thereof Pending CN104099091A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105969347A (en) * 2016-05-31 2016-09-28 吉林大学 Method for acquiring up-conversion white light
CN106085423A (en) * 2016-05-31 2016-11-09 吉林大学 Conversion of white light material C aF in one2: Yb3+/ Eu3+/ Y3+
CN113403065A (en) * 2021-04-30 2021-09-17 河北大学 Fluoride-based stress luminescent material, preparation method and application thereof
CN113403065B (en) * 2021-04-30 2022-11-18 河北大学 Fluoride-based stress luminescent material, preparation method and application thereof

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