CN104650912A - Neodymium-doped lanthanum phosphate salt glass up-conversion luminescent material, preparation method and application thereof - Google Patents
Neodymium-doped lanthanum phosphate salt glass up-conversion luminescent material, preparation method and application thereof Download PDFInfo
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- CN104650912A CN104650912A CN201310578188.3A CN201310578188A CN104650912A CN 104650912 A CN104650912 A CN 104650912A CN 201310578188 A CN201310578188 A CN 201310578188A CN 104650912 A CN104650912 A CN 104650912A
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- phosphate salt
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Abstract
The invention relates to a neodymium-doped lanthanum phosphate salt glass up-conversion luminescent material, a chemical formula is La1-xPO4: xNd<3+>, wherein, x is 0.002-0.03. In a photoluminescence spectrum of the neodymium-doped lanthanum phosphate salt glass up-conversion luminescent material, the excitation wavelength of the neodymium-doped lanthanum phosphate salt glass up-conversion luminescent material is 586nm, a luminescence peak is formed by transition radiation of Nd<3+>ion 2P3/2-4I15/2 in a 469nm wavelength zone, and the luminescent material can be taken as a blue light luminescent material. The invention also provides a preparation method of the neodymium-doped lanthanum phosphate salt glass up-conversion luminescent material and an organic light-emitting diode by using the neodymium-doped lanthanum phosphate salt glass up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of neodymium doped lanthanum phosphate salt glass up-conversion luminescent material, preparation method and Organic Light Emitting Diode.
Background technology
Organic Light Emitting Diode (OLED) because unit construction is simple, the characteristic such as cheap, the luminous of production cost, reaction times is short, flexible, and obtain a very wide range of application.But because the OLED blue light material obtaining stability and high efficiency is at present more difficult, significantly limit the development of white light OLED device and light source industry.
Upconverting fluorescent material can launch visible ray under long wave (as infrared) radiation excitation, even UV-light, is with a wide range of applications in the field such as optical fiber communication technology, fibre amplifier, 3 D stereo display, biomolecules fluorescence labelling, infrared detective.But, can by infrared, the long-wave radiations such as red-green glow inspire the neodymium doped lanthanum phosphate salt glass up-conversion luminescent material of blue emission, have not yet to see report.
Summary of the invention
Based on this, being necessary to provide a kind of can inspire the neodymium doped lanthanum phosphate salt glass up-conversion luminescent material of blue light, preparation method by long-wave radiation and use the Organic Light Emitting Diode of this neodymium doped lanthanum phosphate salt glass up-conversion luminescent material.
A kind of neodymium doped lanthanum phosphate salt glass up-conversion luminescent material, described chemical general formula is La
1-xpO
4: xNd
3+, wherein, x is 0.002 ~ 0.03.
Described x is 0.01.
A preparation method for neodymium doped lanthanum phosphate salt glass up-conversion luminescent material, comprises the following steps:
Step one, according to La
1-xpO
4: xNd
3+the stoichiometric ratio of each element takes La
2o
3, P
2o
5and Nd
2o
3powder, wherein x is 0.002 ~ 0.03;
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 150 DEG C ~ 400 DEG C, then be incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is La
1-xpO
4: xNd
3+neodymium doped lanthanum phosphate salt glass up-conversion luminescent material.
Described La
2o
3, P
2o
5and Nd
2o
3the each component molar of powder is than being (0.97 ~ 0.998): 1:(0.002 ~ 0.03).
Described La
2o
3, P
2o
5and Nd
2o
3the each component molar of powder is than being 0.99:1:0.01.
Described in described step 2, mixing is that described powder is ground 20 minutes ~ 60 minutes in corundum alms bowl.
By the calcination 3 hours at 900 DEG C of described presoma in described step 3.
Cooling temperature in described step 4 is 250 DEG C, and soaking time is 2 hours.
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 neodymium doped lanthanum phosphate salt glass up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of described neodymium doped lanthanum phosphate salt glass up-conversion luminescent material is La
1-xpO
4: xNd
3+, wherein, x is 0.002 ~ 0.03.
Described x is 0.01.
The preparation method of above-mentioned neodymium doped lanthanum phosphate salt glass up-conversion luminescent material is comparatively simple, and cost is lower, produces, comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of the neodymium doped lanthanum phosphate salt glass up-conversion luminescent material of preparation, the excitation wavelength of neodymium doped lanthanum phosphate salt glass 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 doped lanthanum phosphate salt glass up-conversion luminescent material prepared by embodiment 1.
Fig. 3 is the XRD figure of neodymium doped lanthanum phosphate salt glass 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 doped lanthanum phosphate salt glass up-conversion luminescent material material.
Embodiment
Below in conjunction with the drawings and specific embodiments, neodymium doped lanthanum phosphate salt glass up-conversion luminescent material and preparation method thereof is illustrated further.
The neodymium doped lanthanum phosphate salt glass up-conversion luminescent material of one embodiment, its chemical formula is La
1-xpO
4: xNd
3+, wherein, x is 0.002 ~ 0.03.
Preferably, x is 0.01.
The excitation wavelength of this neodymium doped lanthanum phosphate salt glass 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.The present invention also provides the preparation method of this neodymium doped lanthanum phosphate salt glass up-conversion luminescent material and uses the Organic Light Emitting Diode of this neodymium doped lanthanum phosphate salt glass up-conversion luminescent material.
The preparation method of above-mentioned neodymium doped lanthanum phosphate salt glass up-conversion luminescent material, comprises the following steps:
Step S11 is according to La
1-xpO
4: xNd
3+the stoichiometric ratio of each element takes La
2o
3, P
2o
5and Nd
2o
3powder, wherein, x is 0.002 ~ 0.03.
In this step, described La
2o
3, P
2o
5and Nd
2o
3the each component molar of powder is than being (0.97 ~ 0.998): 1:(0.002 ~ 0.03).
In this step, preferred La
2o
3, P
2o
5and Nd
2o
3the each component molar of powder is than being 0.99:1:0.01.
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 150 DEG C ~ 400 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 La
1-xpO
4: xNd
3+, wherein, x is 0.002 ~ 0.03.
Preferably, the precursor after process in step S15 is cooled to 250 DEG C, then is incubated 2 hours.
Preferably, x is 0.01.
The preparation method of above-mentioned neodymium doped lanthanum phosphate salt glass up-conversion luminescent material is comparatively simple, and cost is lower, produces, comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of the neodymium doped lanthanum phosphate salt glass up-conversion luminescent material of preparation, the excitation wavelength of neodymium doped lanthanum phosphate salt glass 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 doped lanthanum phosphate salt glass up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of neodymium doped lanthanum phosphate salt glass up-conversion luminescent material is La
1-xpO
4: xNd
3+, wherein x is 0., 002 ~ 0.03, and the organic luminous layer 3 in this device sends ruddiness, and part ruddiness excites in transparent encapsulated layer 5 and is dispersed with neodymium doped lanthanum phosphate salt glass up-conversion luminescent material 6 and sends blue light, and remaining part is red just blendes together white light with blue light.
Be specific embodiment below.
Embodiment 1
Select purity be 99.99% powder, by La
2o
3, P
2o
5and Nd
2o
3the each component of powder is 0.99mmol by molar fraction, 1mmol 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 200 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 La
0.99pO
4: 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 doped lanthanum phosphate salt glass up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of neodymium doped lanthanum phosphate salt glass up-conversion luminescent material is La
0.99pO
4: 0.01Nd
3+.
Refer to Fig. 2, Figure 2 shows that the photoluminescence spectra figure of the neodymium doped lanthanum phosphate salt glass up-conversion luminescent material obtained.As seen from Figure 2, the excitation wavelength of the neodymium doped lanthanum phosphate salt glass up-conversion luminescent material that the present embodiment obtains is 586nm, in 469nm wavelength zone by Nd
3+ion
2p
3/2→
4i
15/2transition radiation formed glow peak, this neodymium doped lanthanum phosphate salt glass 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 neodymium doped lanthanum phosphate salt glass up-conversion luminescent material prepared by enforcement 1, test comparison standard P DF card.As can be seen from Figure 3, all diffraction peaks are all the characteristic peaks that lanthanum orthophosphate is relevant, do not occur the diffraction peak of doped element and other impurity, prove that doped element is the lattice entering lanthanum orthophosphate.
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 doped lanthanum phosphate salt glass up-conversion luminescent material, and curve 2 is not doped with the contrast of neodymium doped lanthanum phosphate salt glass 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 La
2o
3, P
2o
5and Nd
2o
3the each component of powder is 0.97mmol by molar fraction, 1mmol 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 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 La
0.97pO
4: 0.03Nd
3+up-conversion phosphor.
Embodiment 3
Select purity be 99.99% powder, by La
2o
3, P
2o
5and Nd
2o
3the each component of powder is 0.998mmol by molar fraction, 1mmol 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 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 La
0.998pO
4: 0.002Nd
3+up-conversion phosphor.
Embodiment 4
Select purity be 99.99% powder, by La
2o
3, P
2o
5and Nd
2o
3the each component of powder is 0.98mmol by molar fraction, 1mmol and 0.02mmol 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, after pulverizing, chemical general formula La can be obtained
0.98pO
4: 0.02Nd
3+up-conversion phosphor.
Embodiment 5
Select purity be 99.99% powder, by La
2o
3, P
2o
5and Nd
2o
3the each component of powder is 0.985mmol by molar fraction, 1mmol and 0.015mmol 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 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 La
0.985pO
4: 0.015Nd
3+up-conversion phosphor.
Embodiment 6
Select purity be 99.99% powder, by La
2o
3, P
2o
5and Nd
2o
3the each component of powder is 0.992mmol by molar fraction, 1mmol and 0.008mmol 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 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 La
0.992pO
4: 0.008Nd
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 doped lanthanum phosphate salt glass up-conversion luminescent material, is characterized in that, its chemical general formula is La
1-xpO
4: xNd
3+, wherein, x is 0.002 ~ 0.03.
2. neodymium doped lanthanum phosphate salt glass up-conversion luminescent material according to claim 1, it is characterized in that, described x is 0.01.
3. a preparation method for neodymium doped lanthanum phosphate salt glass up-conversion luminescent material, is characterized in that, comprise the following steps:
Step one, according to La
1-xpO
4: xNd
3+the stoichiometric ratio of each element takes La
2o
3, P
2o
5and Nd
2o
3powder, wherein x is 0.002 ~ 0.03;
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 150 DEG C ~ 400 DEG C, then be incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is La
1-xpO
4: xNd
3+neodymium doped lanthanum phosphate salt glass up-conversion luminescent material.
4. the preparation method of neodymium doped lanthanum phosphate salt glass up-conversion luminescent material according to claim 3, is characterized in that, described La
2o
3, P
2o
5and Nd
2o
3the each component molar of powder is than being (0.97 ~ 0.998): 1:(0.002 ~ 0.03).
5. the preparation method of neodymium doped lanthanum phosphate salt glass up-conversion luminescent material according to claim 3, is characterized in that, described La
2o
3, P
2o
5and Nd
2o
3the each component molar of powder is than being 0.99:1:0.01.
6. the preparation method of neodymium doped lanthanum phosphate salt glass 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 doped lanthanum phosphate salt glass up-conversion luminescent material according to claim 3, is characterized in that, by the calcination 3 hours at 900 DEG C of described presoma in step 3.
8. the preparation method of neodymium doped lanthanum phosphate salt glass up-conversion luminescent material according to claim 3, it is characterized in that, the cooling temperature in step 4 is 200 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 doped lanthanum phosphate salt glass up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of described neodymium doped lanthanum phosphate salt glass up-conversion luminescent material is La
1-xpO
4: xNd
3+, wherein, x is 0.002 ~ 0.03.
10. Organic Light Emitting Diode according to claim 9, is characterized in that, described x is 0.01.
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|---|---|---|---|
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|---|---|---|---|
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| CN201310578188.3A Pending CN104650912A (en) | 2013-11-18 | 2013-11-18 | Neodymium-doped lanthanum phosphate salt glass up-conversion luminescent material, preparation method and application thereof |
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Application publication date: 20150527 |