CN104119890A - Praseodymium samarium co-doped lead fluoride up-conversion luminescent material and preparation method and application thereof - Google Patents
Praseodymium samarium co-doped lead fluoride up-conversion luminescent material and preparation method and application thereof Download PDFInfo
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- CN104119890A CN104119890A CN201310150188.3A CN201310150188A CN104119890A CN 104119890 A CN104119890 A CN 104119890A CN 201310150188 A CN201310150188 A CN 201310150188A CN 104119890 A CN104119890 A CN 104119890A
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- luminescent material
- conversion luminescent
- codoped
- samarium
- praseodymium
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Abstract
A praseodymium samarium co-doped lead fluoride up-conversion luminescent material has the following chemical general formula of PbF4:xPr<3+>, ySm<3+>, wherein x is 0.01-0.08 and y is 0.01-0.06. In a photoluminescence spectrum of the praseodymium samarium co-doped lead fluoride up-conversion luminescent material, the excitation wavelength of the praseodymium samarium co-doped lead fluoride up-conversion luminescent material is 578 nm, in a wavelength region of 483 nm, luminescence peaks can be produced by transition radiation from <3>P0 to <3>H4 of Pr<3+> ions, and the praseodymium samarium co-doped lead fluoride up-conversion luminescent material can be used as a blue light luminescent material. The invention also provides a preparation method of the praseodymium samarium co-doped lead fluoride up-conversion luminescent material, and organic light-emitting diodes using the praseodymium samarium co-doped lead fluoride up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of praseodymium samarium codoped plumbous fluoride 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 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 praseodymium samarium codoped plumbous fluoride 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 be inspired praseodymium samarium codoped plumbous fluoride up-conversion luminescent material, the preparation method of blue light and be used the Organic Light Emitting Diode of this praseodymium samarium codoped plumbous fluoride up-conversion luminescent material by long-wave radiation.
A kind of praseodymium samarium codoped plumbous fluoride up-conversion luminescent material, its chemical formula is PbF
4: xPr
3+, ySm
3+, wherein, x is that 0.01～0.08, y is 0.01～0.06.
Described x is that 0.05, y is 0.03.
A preparation method for praseodymium samarium codoped plumbous fluoride up-conversion luminescent material, comprises the following steps:
Step 1, according to PbF
4: xPr
3+, ySm
3+the stoichiometric ratio of each element takes PbF
4, PrF
3and SmF
3powder, wherein, x is that 0.01～0.08, y is 0.01～0.06;
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～1100 DEG C of the presoma in described step 2,
Step 4, precursor after treatment in described step 3 is cooled to 100 DEG C～300 DEG C, then is incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is PbF
4: xPr
3+, ySm
3+praseodymium samarium codoped plumbous fluoride up-conversion luminescent material.
Described PbF
4, PrF
3and SmF
3the each component mol ratio of powder is (0.86～0.98): (0.01～0.08): (0.01～0.06).
Described PbF
4, PrF
3and SmF
3the each component mol ratio of powder is 0.92:0.05:0.03.
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 200 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, in described transparent encapsulated layer, be dispersed with praseodymium samarium codoped plumbous fluoride up-conversion luminescent material, the chemical formula of described praseodymium samarium codoped plumbous fluoride up-conversion luminescent material is PbF
4: xPr
3+, ySm
3+, wherein, x is that 0.01～0.08, y is 0.01～0.06.
X is that 0.05, y is 0.03.
The preparation method of above-mentioned praseodymium samarium codoped plumbous fluoride 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 praseodymium samarium codoped plumbous fluoride up-conversion luminescent material of preparation, the excitation wavelength of praseodymium samarium codoped plumbous fluoride up-conversion luminescent material is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition 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 praseodymium samarium codoped plumbous fluoride up-conversion luminescent material prepared of embodiment 1.
Fig. 3 is the Raman spectrum of the praseodymium samarium codoped plumbous fluoride up-conversion luminescent material 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 praseodymium samarium codoped plumbous fluoride up-conversion luminescent material.
Embodiment
Below in conjunction with the drawings and specific embodiments, praseodymium samarium codoped plumbous fluoride up-conversion luminescent material and preparation method thereof is further illustrated.
The praseodymium samarium codoped plumbous fluoride up-conversion luminescent material of one embodiment, its chemical formula is PbF
4: xPr
3+, ySm
3+, wherein, x is that 0.01～0.08, y is 0.01～0.06.
Preferably, x is that 0.05, y is 0.03.
In the photoluminescence spectra of this praseodymium samarium codoped plumbous fluoride up-conversion luminescent material, the excitation wavelength of praseodymium samarium codoped plumbous fluoride up-conversion luminescent material is 578nm, in the time that material is subject to long wavelength's (as 483nm) radiation, and Pr
3+ion just in
3p
0excited state, then to
3h
4transition, just sends the blue light of 483nm, can be used as blue light emitting material.
The preparation method of above-mentioned praseodymium samarium codoped plumbous fluoride up-conversion luminescent material, comprises the following steps:
Step S11, according to PbF
4: xPr
3+, ySm
3+the stoichiometric ratio of each element takes PbF
4, PrF
3and SmF
3powder, wherein, x is that 0.01～0.08, y is 0.01～0.06.
In this step, described PbF
4, PrF
3and SmF
3the each component mol ratio of powder is (0.86～0.98): (0.01～0.08): (0.01～0.06).
In this step, preferred, PbF
4, PrF
3and SmF
3the each component mol ratio of powder is 0.92:0.05:0.03.
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～1100 DEG C,
Preferably, presoma calcination 3 hours at 950 DEG C.
Step S17, will be cooled to 100 DEG C～300 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 PbF
4: xPr
3+, ySm
3+, wherein, x is that 0.01～0.08, y is 0.01～0.06.
Preferably, precursor after treatment in step S15 is cooled to 200 DEG C, then is incubated 2 hours.
The preparation method of above-mentioned praseodymium samarium codoped plumbous fluoride 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 praseodymium samarium codoped plumbous fluoride up-conversion luminescent material of preparation, the excitation wavelength of praseodymium samarium codoped plumbous fluoride up-conversion luminescent material is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition 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 praseodymium samarium codoped plumbous fluoride up-conversion luminescent material 6, the chemical formula of praseodymium samarium codoped plumbous fluoride up-conversion luminescent material is PbF
4: xPr
3+, ySm
3+, wherein, x is 0.01～0.08, y is 0.01～0.06, 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 praseodymium samarium codoped plumbous fluoride up-conversion luminescent material 6 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 the PbF of 0.92mmol
4, the PrF of 0.05mmol
3smF with 0.03mmol
3powder grinds and it was evenly mixed in 40 minutes in corundum mortar, and then then calcination 3 hours at 950 DEG C in retort furnace is cooled to 200 DEG C of insulations 2 hours, then furnace cooling takes out to room temperature, obtains block materials, and after pulverizing, can obtain chemical general formula is PbF
4: 0.05Pr
3+, 0.03Sm
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 thulium doped tellurate changing luminous material 6 on glass, the chemical formula of thulium doped with fluorine silex glass up-conversion luminescent material is PbF
4: 0.05Pr
3+, 0.03Sm
3+.
Refer to Fig. 2, Figure 2 shows that the photoluminescence spectra figure of the praseodymium samarium codoped plumbous fluoride up-conversion luminescent material obtaining.As seen from Figure 2, the excitation wavelength of the praseodymium samarium codoped plumbous fluoride up-conversion luminescent material that curve 1 the present embodiment obtains is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation form glow peak, this praseodymium samarium codoped plumbous fluoride up-conversion luminescent material can be used as blue light emitting material, curve 2 is the luminescent spectrum figure of ytterbium element of not adulterating, this shows the sample that has increased ytterbium element codoped, send out light wavelength the same, luminous intensity is compared the sample of the ytterbium element that undopes, and has to such an extent that improve significantly.
Refer to Fig. 3, in Fig. 3, curve is the Raman spectrum of implementing the praseodymium samarium codoped plumbous fluoride up-conversion luminescent material of 1 preparation, Raman peaks in figure is depicted as fluorine manosil AS characteristic peak, does not occur the peak of doped element and other impurity, illustrates that doped element and substrate material have formed good bonding.
Refer to Fig. 4, Fig. 4 curve 1 is for forming the spectrogram of the Organic Light Emitting Diode emitting white light doped with praseodymium samarium codoped plumbous fluoride up-conversion luminescent material in transparent encapsulated layer, curve 2 is the not contrast doped with praseodymium samarium codoped plumbous fluoride up-conversion luminescent material in transparent encapsulated layer.In figure, can find out, fluorescent material can, by the red light of long wave, inspire the blue light of shortwave, blendes together white light.
Embodiment 2
Selecting purity is 99.99% powder, by the PbF of 0.98mmol
4, the PrF of 0.01mmol
3smF with 0.01mmol
3powder grinds and it was evenly mixed in 20 minutes in corundum mortar, and then then calcination 3 hours at 800 DEG C in retort furnace is cooled to 250 DEG C of insulations 0.5 hour, then furnace cooling takes out to room temperature, obtains block materials, and after pulverizing, can obtain chemical general formula is PbF
4: 0.01Pr
3+, 0.01Sm
3+up-conversion phosphor.
Embodiment 3
Selecting purity is 99.99% powder, by the PbF of 0.86mmol
4, the PrF of 0.08mmol
3smF with 0.06mmol
3powder grinds and it was evenly mixed in 60 minutes in corundum mortar, and then then calcination 3 hours at 1000 DEG C in retort furnace is cooled to 250 DEG C of insulations 2 hours, then furnace cooling takes out to room temperature, obtains block materials, and after pulverizing, can obtain chemical general formula is PbF
4: 0.08Pr
3+, 0.06Sm
3+up-conversion phosphor.
Embodiment 4
Selecting purity is 99.99% powder, by the PbF of 0.93mmol
4, the PrF of 0.02mmol
3smF with 0.05mmol
3powder grinds and it was evenly mixed in 30 minutes in corundum mortar, and then then calcination 3 hours at 900 DEG C in retort furnace is cooled to 300 DEG C of insulations 0.5 hour, then furnace cooling takes out to room temperature, obtains block materials, and after pulverizing, can obtain chemical general formula is PbF
4: 0.02Pr
3+, 0.05Sm
3+up-conversion phosphor.
Embodiment 5
Selecting purity is 99.99% powder, by the PbF of 0.92mmol
4, the PrF of 0.06mmol
3smF with 0.02mmol
3powder grinds and it was evenly mixed in 60 minutes in corundum mortar, and then then calcination 2 hours at 850 DEG C in retort furnace is cooled to 300 DEG C of insulations 0.5 hour, then furnace cooling takes out to room temperature, obtains block materials, and after pulverizing, can obtain chemical general formula is PbF
4: 0.06Pr
3+, 0.02Sm
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 praseodymium samarium codoped plumbous fluoride up-conversion luminescent material, is characterized in that: its chemical general formula is PbF
4: xPr
3+, ySm
3+, wherein, x is that 0.01～0.08, y is 0.01～0.06.
2. praseodymium samarium codoped plumbous fluoride up-conversion luminescent material according to claim 1, is characterized in that, described x is that 0.05, y is 0.03.
3. a preparation method for praseodymium samarium codoped plumbous fluoride up-conversion luminescent material, is characterized in that, comprises the following steps:
Step 1, according to PbF
4: xPr
3+, ySm
3+the stoichiometric ratio of each element takes PbF
4, PrF
3and SmF
3powder, wherein, x is that 0.01～0.08, y is 0.01～0.06;
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～1100 DEG C of described presoma,
Step 4, precursor after treatment in described step 3 is cooled to 100 DEG C～300 DEG C, then is incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is PbF
4: xPr
3+, ySm
3+praseodymium samarium codoped plumbous fluoride up-conversion luminescent material.
4. the preparation method of praseodymium samarium codoped plumbous fluoride up-conversion luminescent material according to claim 3, is characterized in that described PbF
4, PrF
3and SmF
3the each component mol ratio of powder is (0.86～0.98): (0.01～0.08): (0.01～0.06).
5. the preparation method of praseodymium samarium codoped plumbous fluoride up-conversion luminescent material according to claim 3, is characterized in that described PbF
4, PrF
3and SmF
3the each component mol ratio of powder is 0.92:0.05:0.03.
6. the preparation method of praseodymium samarium codoped plumbous fluoride up-conversion luminescent material according to claim 3, 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 praseodymium samarium codoped plumbous fluoride up-conversion luminescent material according to claim 3, is characterized in that, in step 3 by the calcination 3 hours at 950 DEG C of described presoma.
8. the preparation method of praseodymium samarium codoped plumbous fluoride up-conversion luminescent material according to claim 3, 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, in described transparent encapsulated layer, be dispersed with praseodymium samarium codoped plumbous fluoride up-conversion luminescent material, the chemical formula of described praseodymium samarium codoped plumbous fluoride up-conversion luminescent material is PbF
4: xPr
3+, ySm
3+, wherein, x is that 0.01～0.08, y is 0.01～0.06.
10. Organic Light Emitting Diode according to claim 9, is characterized in that, described x is that 0.05, y is 0.03.
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|---|---|---|---|
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|---|---|---|---|
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|---|---|---|---|
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4032351A (en) * | 1974-07-24 | 1977-06-28 | Auzel Francois F | Rare earth ceramic for frequency conversion of radiation |
| EP0751200A1 (en) * | 1995-06-30 | 1997-01-02 | Agfa-Gevaert N.V. | A radiation image storage screen comprising an alkali metal halide phosphor |
| CN102140344A (en) * | 2010-02-03 | 2011-08-03 | 中国科学院福建物质结构研究所 | Two-mode nanometer fluorescence labelling material based on rare earth doped sodium gadolinium fluoride core-shell structure and preparation method thereof |
-
2013
- 2013-04-26 CN CN201310150188.3A patent/CN104119890A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4032351A (en) * | 1974-07-24 | 1977-06-28 | Auzel Francois F | Rare earth ceramic for frequency conversion of radiation |
| EP0751200A1 (en) * | 1995-06-30 | 1997-01-02 | Agfa-Gevaert N.V. | A radiation image storage screen comprising an alkali metal halide phosphor |
| CN102140344A (en) * | 2010-02-03 | 2011-08-03 | 中国科学院福建物质结构研究所 | Two-mode nanometer fluorescence labelling material based on rare earth doped sodium gadolinium fluoride core-shell structure and preparation method thereof |
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Application publication date: 20141029 |