CN104650910A - Praseodymium-doped cerium phosphate up-conversion luminescent material, and preparation method and application thereof - Google Patents
Praseodymium-doped cerium phosphate up-conversion luminescent material, and preparation method and application thereof Download PDFInfo
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- CN104650910A CN104650910A CN201310576873.2A CN201310576873A CN104650910A CN 104650910 A CN104650910 A CN 104650910A CN 201310576873 A CN201310576873 A CN 201310576873A CN 104650910 A CN104650910 A CN 104650910A
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Abstract
The invention provides a praseodymium-doped cerium phosphate up-conversion luminescent material. The material has the chemical formula of Ce1-xPO4: xPr<3+>, wherein x is in a range of 0.002 to 0.03. According to the photoluminescence spectrum of the praseodymium-doped cerium phosphate up-conversion luminescent material, the excitation wavelength of the material is 578 nm, transition radiation of Pr3+ ions from 3P0 to 3H4 in the region of 483-nm wavelength leads to formation of luminescent peaks, so the material can be used as a blue-light emitting material. The invention also provides a preparation method for the praseodymium-doped cerium phosphate up-conversion luminescent material and an organic light emitting diode using the praseodymium-doped cerium phosphate up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of praseodymium doped Cerium monophosphate 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 praseodymium doped Cerium monophosphate 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 praseodymium doped Cerium monophosphate glass up-conversion luminescent material of blue light, preparation method by long-wave radiation and use the Organic Light Emitting Diode of this praseodymium doped Cerium monophosphate glass up-conversion luminescent material.
A kind of praseodymium doped Cerium monophosphate glass up-conversion luminescent material, its chemical general formula is Ce
1-xpO
4: xPr
3+, wherein, x is 0.002 ~ 0.03.
Described x is 0.01.
A preparation method for praseodymium doped Cerium monophosphate glass up-conversion luminescent material, comprises the following steps:
Described step one, according to Ce
1-xpO
4: xPr
3+the stoichiometric ratio of each element takes Ce
2o
3, P
2o
5and Pr
2o
3powder, wherein, x is 0.002 ~ 0.03;
Described step 2, the powder taken mixed obtain presoma in described step one;
Described step 3, by the calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C of described presoma,
Described 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 Ce
1-xpO
4: xPr
3+praseodymium doped Cerium monophosphate glass up-conversion luminescent material.
Described Ce
2o
3, P
2o
5and Pr
2o
3the each component molar of powder is than being (0.97 ~ 0.998): 1:(0.002 ~ 0.03).
Described Ce
2o
3, P
2o
5and Pr
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 950 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 praseodymium doped Cerium monophosphate glass up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of described praseodymium doped Cerium monophosphate glass up-conversion luminescent material is Ce
1-xpO
4: xPr
3+, wherein, x is 0.002 ~ 0.03.
Described x is 0.01.
The preparation method of above-mentioned praseodymium doped Cerium monophosphate 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 praseodymium doped Cerium monophosphate glass up-conversion luminescent material of preparation, the excitation wavelength of praseodymium doped Cerium monophosphate glass up-conversion luminescent material is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation formed glow peak, can as blue light emitting material.
Accompanying drawing explanation
Fig. 1 is the structural representation of the Organic Light Emitting Diode of an embodiment.
Fig. 2 is the photoluminescence spectrogram of praseodymium doped Cerium monophosphate glass up-conversion luminescent material prepared by embodiment 1.
Fig. 3 is the XRD figure of praseodymium doped Cerium monophosphate 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 praseodymium doped Cerium monophosphate glass up-conversion luminescent material.
Embodiment
Below in conjunction with the drawings and specific embodiments, praseodymium doped Cerium monophosphate glass up-conversion luminescent material and preparation method thereof is illustrated further.
The praseodymium doped Cerium monophosphate glass up-conversion luminescent material of one embodiment, its chemical formula is Ce
1-xpO
4: xPr
3+, wherein, x is 0.002 ~ 0.03.
Preferably, x is 0.01.
In the photoluminescence spectra of this praseodymium doped Cerium monophosphate glass up-conversion luminescent material, the excitation wavelength of praseodymium doped Cerium monophosphate glass up-conversion luminescent material is 578nm, when material is subject to the radiation of long wavelength (as 578nm) time, and Pr
3+ion has just been in
3p
0excited state, then to
3h
4transition, just sends the blue light of 483nm, can as blue light emitting material.
The preparation method of above-mentioned praseodymium doped Cerium monophosphate glass up-conversion luminescent material, comprises the following steps:
Step S11, according to Ce
1-xpO
4: xPr
3+the stoichiometric ratio of each element takes Ce
2o
3, P
2o
5and Pr
2o
3powder, wherein, x is 0.002 ~ 0.03.
In this step, described Ce
2o
3, P
2o
5and Pr
2o
3powder, wherein, x is each component molar ratio of 0.002 ~ 0.03 powder is (0.97 ~ 0.998): 1:(0.002 ~ 0.03).
In this step, preferred Ce
2o
3, P
2o
5and Pr
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 100 DEG C ~ 300 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 Ce
1-xpO
4: xPr
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.
The preparation method of above-mentioned praseodymium doped Cerium monophosphate 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 praseodymium doped Cerium monophosphate glass up-conversion luminescent material of preparation, the excitation wavelength of praseodymium doped Cerium monophosphate glass up-conversion luminescent material is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition 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.Praseodymium doped Cerium monophosphate glass up-conversion luminescent material 6 is dispersed with, the chemical formula Ce of praseodymium doped Cerium monophosphate glass up-conversion luminescent material in transparent encapsulated layer 5
1-xpO
4: xPr
3+, wherein, x is 0.002 ~ 0.03, and the 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 praseodymium doped Cerium monophosphate glass 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 Ce
2o
3, P
2o
5and Pr
2o
3the each component of powder is respectively 0.99mmol by mole number, 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 Ce
0.99pO
4: 0.01Pr
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 praseodymium doped Cerium monophosphate glass up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of praseodymium doped Cerium monophosphate glass up-conversion luminescent material is Ce
0.99pO
4: 0.01Pr
3+.
Refer to Fig. 2, Figure 2 shows that the photoluminescence spectra figure of the praseodymium doped Cerium monophosphate glass up-conversion luminescent material obtained.As seen from Figure 2, the excitation wavelength of the praseodymium doped Cerium monophosphate glass up-conversion luminescent material that the present embodiment obtains is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation formed glow peak, this praseodymium doped Cerium monophosphate 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 praseodymium doped Cerium monophosphate 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 Cerium monophosphate is relevant, do not occur the diffraction peak of doped element and other impurity, prove that doped element is the lattice entering Cerium monophosphate.
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 praseodymium doped Cerium monophosphate glass up-conversion luminescent material, and curve 2 is not doped with the contrast of praseodymium doped Cerium monophosphate glass up-conversion luminescent 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 Ce
2o
3, P
2o
5and Pr
2o
3the each component of powder is respectively as 0.97mmol by mole number, 1mmol and 0.03mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, 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, and obtain block materials, can obtain chemical general formula after pulverizing is Ce
0.97pO
4: 0.03Pr
3+up-conversion phosphor.
Embodiment 3
Select purity be 99.99% powder, by Ce
2o
3, P
2o
5and Pr
2o
3the each component of powder is respectively 0.998mmol by mole number, 1mmol and 0.002mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 60 minutes, 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, and obtain block materials, can obtain chemical general formula after pulverizing is Ce
0.998pO
4: 0.002Pr
3+up-conversion phosphor.
Embodiment 4
Select purity be 99.99% powder, by Ce
2o
3, P
2o
5and Pr
2o
3the each component of powder is respectively 0.998mmol by mole number, 1mmol and 0.002mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 40 minutes, 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, and obtain block materials, can obtain chemical general formula after pulverizing is Ce
0.98pO
4: 0.02Pr
3+up-conversion phosphor.
Embodiment 5
Select purity be 99.99% powder, by Ce
2o
3, P
2o
5and Pr
2o
3the each component of powder is respectively 0.985mmol by mole number, 1mmol and 0.015mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, 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, and obtain block materials, can obtain chemical general formula after pulverizing is Ce
0.985pO
4: 0.015Pr
3+up-conversion phosphor.
Embodiment 6
Select purity be 99.99% powder, by Ce
2o
3, P
2o
5and Pr
2o
3the each component of powder is respectively 0.992mmol by mole number, 1mmol and 0.008mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 60 minutes, 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, and obtain block materials, can obtain chemical general formula after pulverizing is Ce
0.992pO
4: 0.008Pr
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 praseodymium doped Cerium monophosphate glass up-conversion luminescent material, is characterized in that, its chemical general formula is Ce
1-xpO
4: xPr
3+, wherein, x is 0.002 ~ 0.03.
2. praseodymium doped Cerium monophosphate glass up-conversion luminescent material according to claim 1, it is characterized in that, described x is 0.01.
3. a preparation method for praseodymium doped Cerium monophosphate glass up-conversion luminescent material, is characterized in that, comprise the following steps:
Step one, according to Ce
1-xpO
4: xPr
3+the stoichiometric ratio of each element takes Ce
2o
3, P
2o
5and Pr
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 100 DEG C ~ 300 DEG C, then be incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is Ce
1-xpO
4: xPr
3+praseodymium doped Cerium monophosphate glass up-conversion luminescent material.
4. the preparation method of praseodymium doped Cerium monophosphate glass up-conversion luminescent material according to claim 3, is characterized in that, described Ce
2o
3, P
2o
5and Pr
2o
3the each component molar of powder is than being (0.97 ~ 0.998): 1:(0.002 ~ 0.03).
5. the preparation method of praseodymium doped Cerium monophosphate glass up-conversion luminescent material according to claim 3, is characterized in that, described Ce
2o
3, P
2o
5and Pr
2o
3the each component molar of powder is than being 0.99:1:0.01.
6. the preparation method of praseodymium doped Cerium monophosphate 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 praseodymium doped Cerium monophosphate glass 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 praseodymium doped Cerium monophosphate glass 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 praseodymium doped Cerium monophosphate glass up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of described praseodymium doped Cerium monophosphate glass up-conversion luminescent material is Ce
1-xpO
4: xPr
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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484844A (en) * | 2020-05-18 | 2020-08-04 | 广东拾传拾美新材料有限公司 | Calcium carbonate-calcium silicate up-conversion fluorescent powder and preparation method thereof |
-
2013
- 2013-11-18 CN CN201310576873.2A patent/CN104650910A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484844A (en) * | 2020-05-18 | 2020-08-04 | 广东拾传拾美新材料有限公司 | Calcium carbonate-calcium silicate up-conversion fluorescent powder and preparation method thereof |
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