CN104178166A - Praseodymium-doped sulfo lanthanum gallate up-conversion luminescent materials, and preparing method and applications thereof - Google Patents
Praseodymium-doped sulfo lanthanum gallate up-conversion luminescent materials, and preparing method and applications thereof Download PDFInfo
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- CN104178166A CN104178166A CN201310194875.5A CN201310194875A CN104178166A CN 104178166 A CN104178166 A CN 104178166A CN 201310194875 A CN201310194875 A CN 201310194875A CN 104178166 A CN104178166 A CN 104178166A
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Abstract
A praseodymium-doped sulfo lanthanum gallate up-conversion luminescent materials are provided. The chemical formula of the up-conversion luminescent materials is LaGaS3:xPr<3+>, wherein the x is 0.002-0.06. In a photoluminescence spectrum of the up-conversion luminescent material, the excitation wavelength of the up-conversion luminescent material is 578 nm, and a luminescence peak is formed at 483 nm by transition radiation from the 3P0 to the 3H4 of the Pr<3+>. The up-conversion luminescent material can be adopted as blue luminescent material. A preparing method of the up-conversion luminescent material and an organic light emitting diode adopting the up-conversion luminescent material are also provided.
Description
Technical field
The present invention relates to a kind of praseodymium doping thiogallate lanthanum 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, and obtained the utmost point, apply widely.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 doping thiogallate lanthanum 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 doping thiogallate lanthanum up-conversion luminescent material, the preparation method of blue light and be used the Organic Light Emitting Diode of this praseodymium doping thiogallate lanthanum up-conversion luminescent material by long-wave radiation.
A praseodymium doping thiogallate lanthanum up-conversion luminescent material, its chemical formula is LaGaS
3: xPr
3+, wherein, x is 0.002～0.06.
Described x is 0.03.
A preparation method for praseodymium doping thiogallate lanthanum up-conversion luminescent material, comprises the following steps
Step 1, according to LaGaS
3: xPr
3+the stoichiometric ratio of each element takes La
2s
3, Ga
2s
3and Pr
2s
3powder, wherein, x is 0.002～0.06;
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 ℃～1100 ℃ of the presoma in described step 2,
Step 4, the precursor after processing in described step 3 is cooled to 100 ℃～300 ℃, then is incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is LaGaS
3: xPr
3+praseodymium doping thiogallate lanthanum up-conversion luminescent material.
Described La
2s
3, Ga
2s
3and Pr
2s
3each component mol ratio of powder is (0.94～0.998): 1:(0.002～0.06).
Described La
2s
3, Ga
2s
3and Pr
2s
3each component mol ratio of powder is 0.97:1:0.03.
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 ℃ of described presoma.
Cooling temperature in step 4 is 200 ℃, 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 praseodymium doping thiogallate lanthanum up-conversion luminescent material, the chemical formula of described praseodymium doping thiogallate lanthanum up-conversion luminescent material is LaGaS
3: xPr
3+, wherein, x is 0.002～0.06.
Described x is 0.03.
The preparation method of above-mentioned praseodymium doping thiogallate lanthanum 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 doping thiogallate lanthanum up-conversion luminescent material of preparation, the excitation wavelength of praseodymium doping thiogallate lanthanum 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.
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 the praseodymium doping thiogallate lanthanum up-conversion luminescent material of embodiment 1 preparation.
Fig. 3 is the Raman spectrum of the praseodymium doping thiogallate lanthanum up-conversion luminescent material of embodiment 1 preparation.
Fig. 4 forms the spectrogram of the Organic Light Emitting Diode emitting white light doped with praseodymium doping thiogallate lanthanum up-conversion luminescent material material in the transparent encapsulated layer of embodiment 1 preparation.
Embodiment
Below in conjunction with the drawings and specific embodiments, praseodymium doping thiogallate lanthanum up-conversion luminescent material and preparation method thereof is further illustrated.
The praseodymium doping thiogallate lanthanum up-conversion luminescent material of one embodiment, its chemical formula is LaGaS
3: xPr
3+, wherein, x is 0.002～0.06.
Preferably, x is 0.03.
In the photoluminescence spectra of this praseodymium doping thiogallate lanthanum up-conversion luminescent material, the excitation wavelength of praseodymium doping thiogallate lanthanum up-conversion luminescent material is 578nm, when material is subject to long wavelength's (as 578nm) 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 doping thiogallate lanthanum up-conversion luminescent material, comprises the following steps:
Step S11, according to LaGaS
3: xPr
3+the stoichiometric ratio of each element takes La
2s
3, Ga
2s
3and Pr
2s
3powder, wherein, x is 0.002～0.06.
In this step, described La
2s
3, Ga
2s
3and Pr
2s
3each component mol ratio of powder is (0.94～0.998): 1:(0.002～0.06).
In this step, preferred, La
2s
3, Ga
2s
3and Pr
2s
3each component mol ratio of powder is 0.97:1:0.03.
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 ℃～1100 ℃,
Preferably, presoma calcination 3 hours at 950 ℃.
After step S17, the precursor after will be in step S15 processing, be cooled to 100 ℃～500 ℃, then be incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is LaGaS
3: xPr
3+praseodymium doping thiogallate lanthanum up-conversion luminescent material, wherein, x is 0.002～0.06.
Preferably, the precursor after processing in step S15 is cooled to 200 ℃, then is incubated 2 hours.
The preparation method of above-mentioned praseodymium doping thiogallate lanthanum 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 doping thiogallate lanthanum up-conversion luminescent material of preparation, the excitation wavelength of praseodymium doping thiogallate lanthanum 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 substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the transparent encapsulated layer 5 stacking gradually.In transparent encapsulated layer 5, be dispersed with praseodymium doping thiogallate lanthanum up-conversion luminescent material 6, the chemical formula of praseodymium doping thiogallate lanthanum up-conversion luminescent material is LaGaS
3: xPr
3+, wherein, x is 0.002～0.06, and the 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 doping thiogallate lanthanum 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 La
2s
3, Ga
2s
3and Pr
2s
3each component of powder is 0.97mmol by mole number, 1mmol and 0.03mmol grind and it were evenly mixed in 40 minutes in corundum mortar, then calcination 3 hours at 950 ℃ in retort furnace, then be cooled to 200 ℃ of insulations 2 hours, furnace cooling takes out to room temperature again, obtain block materials, after pulverizing, can obtain chemical general formula is LaGaS
3: 0.03Pr
3+up-conversion phosphor.
Process prepared by Organic Light Emitting Diode
The substrate 1 stacking gradually uses soda-lime glass, negative electrode 2 to use metal A g layer, organic luminous layer 3 to use Ir (piq) 2 (acac) Chinese name to close iridium (III), transparent anode 4 use tin indium oxide ITO two (1-phenyl-isoquinoline 99.9) (methyl ethyl diketones), and transparent encapsulated layer 5 tetrafluoroethylene.In transparent encapsulated layer 5, be dispersed with praseodymium doping thiogallate lanthanum up-conversion luminescent material 6, the chemical formula of praseodymium doping thiogallate lanthanum up-conversion luminescent material is LaGaS
3: 0.03Pr
3+.
Refer to Fig. 2, Figure 2 shows that the photoluminescence spectra figure of the praseodymium doping thiogallate lanthanum up-conversion luminescent material obtaining.As seen from Figure 2, the excitation wavelength of praseodymium that the present embodiment obtains doping thiogallate lanthanum up-conversion luminescent material is 578nm, in 483nm wavelength zone by Pr
3+ion
3p
0→
3h
4transition radiation form glow peak, this praseodymium doping thiogallate lanthanum up-conversion luminescent material can be used as blue light emitting material.
Refer to Fig. 3, in Fig. 3, curve is for implementing the Raman spectrum of the praseodymium doping thiogallate lanthanum up-conversion luminescent material of 1 preparation, Raman peaks in figure is depicted as thiogallate lanthanum characteristic peak, the peak that does not occur 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 form the spectrogram of the Organic Light Emitting Diode emitting white light in transparent encapsulated layer doped with praseodymium doping thiogallate lanthanum up-conversion luminescent material material, and curve 2 be not doped with the adulterate contrast of thiogallate lanthanum up-conversion luminescent material material of praseodymium in transparent encapsulated layer.In figure, can find out, up-conversion luminescent material can inspire the blue light of shortwave by the red light of long wave, after blue light mixes with ruddiness, forms white light.
Embodiment 2
Selecting purity is 99.99% powder, by La
2s
3, Ga
2s
3and Pr
2s
3each component of powder is 0.998mmol by mole number, 1mmol and 0.002mmol grind and it were evenly mixed in 20 minutes in corundum mortar, then calcination 3 hours at 800 ℃ in retort furnace, then be cooled to 250 ℃ of insulations 2 hours, furnace cooling takes out to room temperature again, obtain block materials, after pulverizing, can obtain chemical general formula is LaGaS
3: 0.002Pr
3+up-conversion phosphor.
Embodiment 3
Selecting purity is 99.99% powder, by La
2s
3, Ga
2s
3and Pr
2s
3each component of powder is 0.94mmol by mole number, 1mmol and 0.06mmol grind and it were evenly mixed in 60 minutes in corundum mortar, then calcination 3 hours at 1000 ℃ in retort furnace, then be cooled to 250 ℃ of insulations 2 hours, furnace cooling takes out to room temperature again, obtain block materials, after pulverizing, can obtain chemical general formula is LaGaS
3: 0.06Pr
3+up-conversion phosphor.
Embodiment 4
Selecting purity is 99.99% powder, by La
2s
3, Ga
2s
3and Pr
2s
3each component of powder is 0.99mmol by mole number, 1mmol and 0.01mmol grind and it were evenly mixed in 50 minutes in corundum mortar, then calcination 3 hours at 970 ℃ in retort furnace, then be cooled to 250 ℃ of insulations 2 hours, furnace cooling takes out to room temperature again, obtain block materials, after pulverizing, can obtain chemical general formula is LaGaS
3: 0.01Pr
3+up-conversion phosphor.
Embodiment 5
Selecting purity is 99.99% powder, by La
2s
3, Ga
2s
3and Pr
2s
3each component of powder is 0.96mmol by mole number, 1mmol and 0.04mmol, in corundum mortar, grind and it was evenly mixed in 30 minutes, then calcination 3 hours at 850 ℃ in retort furnace, then be cooled to 250 ℃ of insulations 2 hours, furnace cooling takes out to room temperature again, obtains block materials, and after pulverizing, can obtain chemical general formula is LaGaS
3: 0.04Pr
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 doping thiogallate lanthanum up-conversion luminescent material, is characterized in that: its chemical general formula is LaGaS
3: xPr
3+, wherein, x is 0.002～0.06.
2. praseodymium doping thiogallate lanthanum up-conversion luminescent material according to claim 1, is characterized in that, described x is 0.03.
3. a preparation method for praseodymium doping thiogallate lanthanum up-conversion luminescent material, is characterized in that, comprises the following steps:
Step 1, according to LaGaS
3: xPr
3+the stoichiometric ratio of each element takes La
2s
3, Ga
2s
3and Pr
2s
3powder, wherein, x is 0.002～0.06;
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 ℃～1100 ℃ of described presoma,
Step 4, the precursor after processing in described step 3 is cooled to 100 ℃～300 ℃, then is incubated 0.5 hour～3 hours, cool to room temperature, obtaining chemical general formula is LaGaS
3: xPr
3+praseodymium doping thiogallate lanthanum up-conversion luminescent material.
4. the preparation method of praseodymium doping thiogallate lanthanum up-conversion luminescent material according to claim 3, is characterized in that described La
2s
3, Ga
2s
3and Pr
2s
3each component mol ratio of powder is (0.94～0.998): 1:(0.002～0.06).
5. the preparation method of praseodymium doping thiogallate lanthanum up-conversion luminescent material according to claim 3, is characterized in that described La
2s
3, Ga
2s
3and Pr
2s
3each component mol ratio of powder is 0.97:1:0.03.
6. the preparation method of praseodymium doping thiogallate lanthanum 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 according to claim 3 doping thiogallate lanthanum up-conversion luminescent material, is characterized in that, in step 3 by the calcination 3 hours at 950 ℃ of described presoma.
8. the preparation method of praseodymium doping thiogallate lanthanum up-conversion luminescent material according to claim 3, is characterized in that, the cooling temperature in step 4 is 200 ℃, and soaking time is 2 hours.
9. an Organic Light Emitting Diode, this Organic Light Emitting Diode comprises substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer stacking gradually, it is characterized in that, in described transparent encapsulated layer, be dispersed with praseodymium doping thiogallate lanthanum up-conversion luminescent material, the chemical formula of described praseodymium doping thiogallate lanthanum up-conversion luminescent material is LaGaS
3: xPr
3+, wherein, x is 0.002～0.06.
10. Organic Light Emitting Diode according to claim 9, is characterized in that, described x is 0.03.
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Cited By (2)
| 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 |
| JP2023524178A (en) * | 2020-09-14 | 2023-06-08 | 大連民族大学 | Polyvalent sulfide upconversion luminescence material |
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| 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 |
| JP2023524178A (en) * | 2020-09-14 | 2023-06-08 | 大連民族大学 | Polyvalent sulfide upconversion luminescence material |
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Application publication date: 20141203 |