CN104449681A - Nd/Yb-codoped alkaline earth sulfide up-conversion luminescent material as well as preparation method and application thereof - Google Patents
Nd/Yb-codoped alkaline earth sulfide up-conversion luminescent material as well as preparation method and application thereof Download PDFInfo
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- CN104449681A CN104449681A CN201310442640.3A CN201310442640A CN104449681A CN 104449681 A CN104449681 A CN 104449681A CN 201310442640 A CN201310442640 A CN 201310442640A CN 104449681 A CN104449681 A CN 104449681A
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- alkaline earth
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Abstract
The invention discloses a Nd/Yb-codoped alkaline earth sulfide up-conversion luminescent material having a chemical formula of RS:xYb<3+>, yNd<3+>, wherein x is between 0.005 and 0.05, y is between 0.002 and 0.03, R is at least one of Mg, Ca, Sr and Ba. In the electroluminescence (EL) spectrum of the Nd/Yb-codoped alkaline earth sulfide up-conversion luminescent material, the excitation wavelength of the Nd/Yb-codoped alkaline earth sulfide up-conversion luminescent material is 586nm, a light emission peak is formed by transition radiation of Nd<3+> ion <2>P3/2-><4>I15/2 in a 469nm wavelength region, and therefore the Nd/Yb-codoped alkaline earth sulfide up-conversion luminescent material can be used as a blue light emitting material. The invention further provides a preparation method of the Nd/Yb-codoped alkaline earth sulfide up-conversion luminescent material and an organic light emitting diode using the Nd/Yb-codoped alkaline earth sulfide up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of neodymium ytterbium codoped alkaline earth sulfide 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 neodymium ytterbium codoped alkaline earth sulfide 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 neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material of blue light, preparation method by long-wave radiation and use the Organic Light Emitting Diode of this neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material.
A kind of neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material, its chemical formula is RS:xYb
3+, yNd
3+, wherein, x is 0.005 ~ 0.05, y be 0.002 ~ 0.03, R is magnesium, calcium, at least one in strontium and barium.
Described x is 0.03, y is 0.01.
A preparation method for neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material, comprises the following steps
Step one, according to RS:xYb
3+, yNd
3+the stoichiometric ratio of each element takes RS, Yb
2s
3and Nd
2s
3powder, wherein, x is 0.005 ~ 0.05, y be 0.002 ~ 0.03, R is magnesium, calcium, at least one in strontium and barium;
Step 2, the powder taken mixed obtain presoma in described step one;
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, the precursor after process in described step 3 is cooled to 100 DEG C ~ 300 DEG C, then be incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is RS:xYb
3+, yNd
3+neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material.
Described RS, Yb
2s
3and Nd
2s
3the each component molar of powder is than being (92 ~ 99.3): (0.5 ~ 5): (0.2 ~ 3).
Described RS, Yb
2s
3and Nd
2s
3the each component molar of powder is than being 96:3:1.
Described in step 2, mixing is that described powder is ground 20 minutes ~ 60 minutes in corundum alms bowl.
By the calcination 3 hours at 950 DEG C of described presoma in step 3.
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, it is characterized in that, be dispersed with neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of described neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material is RS:xYb
3+, yNd
3+, wherein, x is 0.005 ~ 0.05, y be 0.002 ~ 0.03, R is magnesium, calcium, at least one in strontium and barium.
Described x is 0.03, y is 0.01.
The preparation method of above-mentioned neodymium ytterbium codoped alkaline earth sulfide 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 neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material of preparation, the excitation wavelength of neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material is 586nm, in 469nm wavelength zone by Nd
3+ion
2p
3/2→
4i
15/2transition 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 neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material prepared by embodiment 1.
Fig. 3 is the XRD figure spectrum of neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material prepared by embodiment 1.
Fig. 4 is the spectrogram forming the Organic Light Emitting Diode emitted white light in the transparent encapsulated layer of embodiment 1 preparation doped with neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material material.
Embodiment
Below in conjunction with the drawings and specific embodiments, neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material and preparation method thereof is illustrated further.
The neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material of one embodiment, its chemical formula is RS:xYb
3+, yNd
3+, wherein, x is 0.005 ~ 0.05, y be 0.002 ~ 0.03, R is magnesium, calcium, at least one in strontium and barium.
Preferably, x is 0.03, y is 0.01.
In the photoluminescence spectra of this neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material, the excitation wavelength of neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material is 586nm, when material is subject to the radiation of long wavelength (as 586nm) time, and Nd
3+ion has just been in
2p
3/2excited state, then to
4i
15/2transition, just sends the blue light of 469nm, can as blue light emitting material.
The preparation method of above-mentioned neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material, comprises the following steps:
Step S11, according to RS:xYb
3+, yNd
3+the stoichiometric ratio of each element takes RS, Yb
2s
3and Nd
2s
3powder, wherein, x is 0.005 ~ 0.05, y be 0.002 ~ 0.03, R is magnesium, calcium, at least one in strontium and barium.
In this step, described RS, Yb
2s
3and Nd
2s
3the each component molar of powder is than being (92 ~ 99.3): (0.5 ~ 5): (0.2 ~ 3).
In this step, preferred RS, Yb
2s
3and Nd
2s
3the each component molar of powder is than being 96:3:1.
Step S13, the powder taken mixed obtain presoma in step S11.
In this step, powder is ground in corundum alms bowl the presoma obtaining mixing for 20 minutes ~ 60 minutes, preferred grinding 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, be cooled to 100 DEG C ~ 500 DEG C by after the precursor after process in step S15, then be incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is RS:xYb
3+, yNd
3+, wherein, x is 0.005 ~ 0.05, y be 0.002 ~ 0.03, R is magnesium, calcium, at least one in strontium and barium.
Preferably, the precursor after process in step S15 is cooled to 250 DEG C, then is incubated 2 hours.
Preferably, described x is 0.03, y is 0.01.
The preparation method of above-mentioned neodymium ytterbium codoped alkaline earth sulfide 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 neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material of preparation, the excitation wavelength of neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material is 586nm, in 469nm wavelength zone by Nd
3+ion
2p
3/2→
4i
15/2transition radiation formed glow peak, can 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.Be dispersed with neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material is RS:xYb
3+, yNd
3+wherein, x is 0.005 ~ 0.05, y is 0.002 ~ 0.03, R is magnesium, calcium, at least one in strontium and barium, 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 alkaline earth sulfide 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, by MgS, Yb
2s
3and Nd
2s
3the each component of powder is 0.96mmol by mole number, 0.03mmol and 0.01mmol grinds and makes its Homogeneous phase mixing in 40 minutes in corundum mortar, then calcination 3 hours at 950 DEG C in retort furnace, then 250 DEG C are cooled to be incubated 2 hours, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is MgS:0.03Yb
3+, 0.01Nd
3+up-conversion phosphor.
Process prepared by Organic Light Emitting Diode
The substrate 1 stacked gradually uses soda-lime glass, negative electrode 2 uses metal A g layer, organic luminous layer 3 uses Ir (piq) 2 (acac) Chinese name (methyl ethyl diketone) closes iridium (III), transparent anode 4 uses tin indium oxide ITO two (1-phenyl-isoquinoline 99.9), and transparent encapsulated layer 5 tetrafluoroethylene.Be dispersed with neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material is MgS: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 sulfide up-conversion luminescent material obtained.As seen from Figure 2, the excitation wavelength of the neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material 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 sulfide up-conversion luminescent material can be used as blue light emitting material, and curve 2 is not containing the comparative example MgS:0.01Nd of Yb element doping
3+, can find out the codoped adding Yb element, the glow peak invariant position of sample, luminous intensity significantly improves.
Refer to Fig. 3, in Fig. 3, curve is the XRD curve of neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material prepared by enforcement 1, contrast PDF card, diffraction peak is depicted as the peak crystallization of alkaline earth sulfide, there is not the diffraction peak of doped element and other impurity, illustrate that the product that this preparation method obtains has good crystalline quality.
Refer to Fig. 4, Fig. 4 curve 1 is the spectrogram forming the Organic Light Emitting Diode emitted white light in transparent encapsulated layer doped with neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material material, and curve 2 is not doped with the contrast of neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material material in transparent encapsulated layer.Can find out in figure, up-conversion luminescent material by the red light of long wave, can inspire the blue light of shortwave, forms white light after blue light mixes with ruddiness.
Embodiment 2
Select purity be 99.99% powder, by MgS, Yb
2s
3and Nd
2s
3the each component of powder is 0.965mmol by mole number, 0.005mmol and 0.03mmol grinds and makes its Homogeneous phase mixing in 20 minutes in corundum mortar, then calcination 3 hours at 800 DEG C in retort furnace, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is MgS:0.005Yb
3+, 0.03Nd
3+up-conversion phosphor.
Embodiment 3
Select purity be 99.99% powder, by MgS, Yb
2s
3and Nd
2s
3the each component of powder is 0.948mmol by mole number, 0.05mmol and 0.002mmol grinds and makes its Homogeneous phase mixing in 60 minutes in corundum mortar, then calcination 0.5 hour at 1000 DEG C in retort furnace, then 500 DEG C are cooled to be incubated 0.5 hour, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is MgS:0.05Yb
3+, 0.002Nd
3+up-conversion phosphor.
Embodiment 4
Select purity be 99.99% powder, by CaS, Yb
2s
3and Nd
2s
3the each component of powder is 0.96mmol by mole number, 0.03mmol and 0.01mmol grinds and makes its Homogeneous phase mixing in 50 minutes in corundum mortar, then calcination 4 hours at 850 DEG C in retort furnace, then 200 DEG C are cooled to be incubated 1 hour, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is CaS:0.03Yb
3+, 0.01Nd
3+up-conversion phosphor.
Embodiment 5
Select purity be 99.99% powder, by CaS, Yb
2s
3and Nd
2s
3the each component of powder is 0.965mmol by mole number, 0.005mmol and 0.03mmol grinds and makes its Homogeneous phase mixing in 30 minutes in corundum mortar, then calcination 5 hours at 900 DEG C in retort furnace, then 400 DEG C are cooled to be incubated 1.5 hours, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is CaS:0.005Yb
3+, 0.03Nd
3+up-conversion phosphor.
Embodiment 6
Select purity be 99.99% powder, by CaS, Yb
2s
3and Nd
2s
3the each component of powder is 0.948mmol by mole number, 0.05mmol and 0.002mmol grinds and makes its Homogeneous phase mixing in 60 minutes in corundum mortar, then calcination 3 hours at 1000 DEG C in retort furnace, then 500 DEG C are cooled to be incubated 0.5 hour, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is CaS:0.05Yb
3+, 0.002Nd
3+up-conversion phosphor.
Embodiment 7
Select purity be 99.99% powder, by SrS, Yb
2s
3and Nd
2s
3the each component of powder is 0.96mmol by mole number, 0.03mmol and 0.01mmol grinds and makes its Homogeneous phase mixing in 40 minutes in corundum mortar, then calcination 3 hours at 950 DEG C in retort furnace, then 250 DEG C are cooled to be incubated 2 hours, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is SrS:0.03Yb
3+, 0.01Nd
3+up-conversion phosphor.
Embodiment 8
Select purity be 99.99% powder, by SrS, Yb
2s
3and Nd
2s
3the each component of powder is 0.965mmol by mole number, 0.005mmol and 0.03mmol grinds and makes its Homogeneous phase mixing in 20 minutes in corundum mortar, then calcination 5 hours at 800 DEG C in retort furnace, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is SrS:0.005Yb
3+, 0.03Nd
3+up-conversion phosphor.
Embodiment 9
Select purity be 99.99% powder, by SrS, Yb
2s
3and Nd
2s
3the each component of powder is 0.948mmol by mole number, 0.05mmol and 0.002mmol grinds and makes its Homogeneous phase mixing in 60 minutes in corundum mortar, then calcination 3 hours at 1000 DEG C in retort furnace, then 500 DEG C are cooled to be incubated 0.5 hour, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is SrS:0.05Yb
3+, 0.002Nd
3+up-conversion phosphor.
Embodiment 10
Select purity be 99.99% powder, by BaS, Yb
2s
3and Nd
2s
3the each component of powder is 0.96mmol by mole number, 0.03mmol and 0.01mmol grinds and makes its Homogeneous phase mixing in 40 minutes in corundum mortar, then calcination 3 hours at 950 DEG C in retort furnace, then 250 DEG C are cooled to be incubated 2 hours, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is BaS:0.03Yb
3+, 0.01Nd
3+up-conversion phosphor.
Embodiment 11
Select purity be 99.99% powder, by BaS, Yb
2s
3and Nd
2s
3the each component of powder is 0.965mmol by mole number, 0.005mmol and 0.03mmol grinds and makes its Homogeneous phase mixing in 20 minutes in corundum mortar, then calcination 5 hours at 800 DEG C in retort furnace, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is BaS:0.005Yb
3+, 0.03Nd
3+up-conversion phosphor.
Embodiment 12
Select purity be 99.99% powder, by BaS, Yb
2s
3and Nd
2s
3the each component of powder is 0.948mmol by mole number, 0.05mmol and 0.002mmol grinds and makes its Homogeneous phase mixing in 60 minutes in corundum mortar, then calcination 3 hours at 1000 DEG C in retort furnace, then 500 DEG C are cooled to be incubated 0.5 hour, furnace cooling takes out to room temperature again, obtain block materials, can obtain chemical general formula after pulverizing is BaS:0.05Yb
3+, 0.002Nd
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 neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material, is characterized in that: its chemical general formula is RS:xYb
3+, yNd
3+, wherein, x is 0.005 ~ 0.05, y be 0.002 ~ 0.03, R is magnesium, calcium, at least one in strontium and barium.
2. neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material according to claim 1, it is characterized in that, described x is 0.03, y is 0.01.
3. a preparation method for neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material, is characterized in that, comprise the following steps:
Step one, according to RS:xYb
3+, yNd
3+the stoichiometric ratio of each element takes RS, Yb
2s
3and Nd
2s
3powder, wherein, x is 0.005 ~ 0.05, y be 0.002 ~ 0.03, R is magnesium, calcium, at least one in strontium and barium;
Step 2, the powder taken mixed obtain presoma in described step one;
Step 3, by the calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C of described presoma,
Step 4, the precursor after process in described step 3 is cooled to 100 DEG C ~ 500 DEG C, then be incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is RS:xYb
3+, yNd
3+neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material.
4. the preparation method of neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material according to claim 3, is characterized in that, described RS, Yb
2s
3and Nd
2s
3the each component molar of powder is than being (92 ~ 99.3): (0.5 ~ 5): (0.2 ~ 3).
5. the preparation method of neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material according to claim 3, is characterized in that, described RS, Yb
2s
3and Nd
2s
3the each component molar of powder is than being 96:3:1.
6. the preparation method of neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material according to claim 3, is characterized in that, described in step 2, mixing is that described powder is ground 20 minutes ~ 60 minutes in corundum alms bowl.
7. the preparation method of neodymium ytterbium codoped alkaline earth sulfide 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.
8. the preparation method of neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material according to claim 3, it 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, be dispersed with neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of described neodymium ytterbium codoped alkaline earth sulfide up-conversion luminescent material is RS:xYb
3+, yNd
3+, wherein, x is 0.005 ~ 0.05, y be 0.002 ~ 0.03, R is magnesium, calcium, at least one in strontium and barium.
10. Organic Light Emitting Diode according to claim 9, is characterized in that, described x is 0.03, y is 0.01.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104877686A (en) * | 2015-06-25 | 2015-09-02 | 西南大学 | Up-converting luminescence material and preparation method thereof |
| CN106433620A (en) * | 2016-06-13 | 2017-02-22 | 郑甘裕 | Alkaline-earth sulfide luminescent material, preparation method and application of material |
-
2013
- 2013-09-25 CN CN201310442640.3A patent/CN104449681A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104877686A (en) * | 2015-06-25 | 2015-09-02 | 西南大学 | Up-converting luminescence material and preparation method thereof |
| CN104877686B (en) * | 2015-06-25 | 2017-05-10 | 西南大学 | Up-converting luminescence material and preparation method thereof |
| CN106433620A (en) * | 2016-06-13 | 2017-02-22 | 郑甘裕 | Alkaline-earth sulfide luminescent material, preparation method and application of material |
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