CN103059854A - Europium-doped calcium lutetium molybdate luminescent film, preparation method thereof, and organic electroluminescent device - Google Patents
Europium-doped calcium lutetium molybdate luminescent film, preparation method thereof, and organic electroluminescent device Download PDFInfo
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- CN103059854A CN103059854A CN201110320324XA CN201110320324A CN103059854A CN 103059854 A CN103059854 A CN 103059854A CN 201110320324X A CN201110320324X A CN 201110320324XA CN 201110320324 A CN201110320324 A CN 201110320324A CN 103059854 A CN103059854 A CN 103059854A
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- moo
- emitting film
- acid lutetium
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- APWKMUZRNGERPD-UHFFFAOYSA-N [Ca].[Lu] Chemical compound [Ca].[Lu] APWKMUZRNGERPD-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 title abstract description 4
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 22
- 239000000126 substance Substances 0.000 claims abstract description 10
- 229910052693 Europium Inorganic materials 0.000 claims description 44
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims description 38
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 34
- 239000011575 calcium Substances 0.000 claims description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 20
- 238000000137 annealing Methods 0.000 claims description 16
- 239000011248 coating agent Substances 0.000 claims description 16
- 238000000576 coating method Methods 0.000 claims description 16
- 238000004544 sputter deposition Methods 0.000 claims description 15
- 238000005401 electroluminescence Methods 0.000 claims description 12
- 239000011159 matrix material Substances 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 239000002019 doping agent Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- 229910052765 Lutetium Inorganic materials 0.000 claims description 7
- 238000007747 plating Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 6
- 150000000918 Europium Chemical class 0.000 claims description 3
- 239000013077 target material Substances 0.000 claims description 3
- 230000007704 transition Effects 0.000 abstract description 8
- 150000002500 ions Chemical class 0.000 abstract description 7
- 238000001228 spectrum Methods 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 43
- 239000011521 glass Substances 0.000 description 13
- 239000000843 powder Substances 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000009832 plasma treatment Methods 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 238000001194 electroluminescence spectrum Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- -1 Rare earth ion Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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Abstract
The invention belongs to the field of photoelectric luminescent films, and discloses a europium-doped calcium lutetium molybdate luminescent film, a preparation method thereof and an organic electroluminescent device. The luminescent film has a chemical general formula of Ca1-x-yLuyMoO4:xEu3+, wherein Eu3+ is doping ions, x value ranges from 0.1 to 0.2, and y value ranges from 0.2-0.6. The europium-doped calcium lutetium molybdate luminescent film (Ca1-x-yLuyMoO4:xEu3+) is obtained by magnetron sputtering equipment. In an electroluminescent spectrum of the luminescent film, a red luminescent peak is mainly composed of electric dipole transitions from 5D0 to 7F2 e with a wavelength of 614 nm and magnetic dipole transitions from 5D0 to 7F1 with a wavelength of 590 nm.
Description
Technical field
The present invention relates to photo-electroluminescence film field, relate in particular to a kind of europium doping molybdic acid lutetium calcium light-emitting film and preparation method thereof.The invention still further relates to a kind of this europium doping molybdic acid lutetium calcium light-emitting film that uses as the organic electroluminescence device of luminescent layer.
Background technology
Thin-film electroluminescent displays (TFELD) since its active illuminating, total solids, shock-resistant, the advantage such as reaction is fast, the visual angle is large, Applicable temperature is wide, operation is simple caused and paid close attention to widely, and development rapidly.At present, the colored material that reaches to panchromatic TFELD of research is the developing direction of this problem.
In recent years, along with the progress of Science and Technology, have higher requirement to photoelectron material in a lot of fields, and novel photoelectron material constantly occurs, and the performance of original material system is constantly improved; Rare earth ion doped molybdate is attractive scintillator and phosphor material powder especially.
Summary of the invention
The object of the invention be to provide a kind of take molybdic acid lutetium calcium as matrix, the europium element is the europium doping molybdic acid lutetium calcium light-emitting film of main luminescence center.
Europium doping molybdic acid lutetium calcium light-emitting film of the present invention, its chemical general formula is Ca
1-x-yLu
yMoO
4: xEu
3+Wherein, Ca
1-x-yLu
yMoO
4Be matrix, Eu
3+Be dopant ion, the span of x is that the span of 0.1～0.2, y is 0.2～0.6; Preferably, the value of x is that the value of 0.15, y is 0.4.
Another goal of the invention of the present invention is to provide the preparation method of above-mentioned europium doping molybdic acid lutetium calcium light-emitting film, and its step of preparation process is as follows:
Step S1 by mass percentage, takes by weighing respectively 14～17.6% CaO, 13.4～40.2% Lu
2O
3, 5.9～11.8% Eu
2O
3And the MoO of surplus
3Raw material, and after even through ground and mixed, at 900～1300 ℃ of lower sintering, make target;
Step S2 packs the target that obtains among the step S1 and substrate in the vacuum cavity of magnetic-controlled sputtering coating equipment into, and the vacuum tightness of vacuum cavity is arranged on 1.0 * 10
-3Pa～1.0 * 10
-5Between the Pa;
Step S3, adjustment magnetron sputtering plating processing parameter is: basic target spacing is 45～95mm, and magnetron sputtering operating pressure 0.2～4Pa, the flow 10～35sccm of argon gas working gas, underlayer temperature are 250 ℃～750 ℃; Then be filmed, obtain film sample;
Step S4 processes 1～3h with the film sample that step S3 obtains in 500～800 ℃ of lower vacuum annealings, and obtaining chemical general formula is Ca
1-x-yLu
yMoO
4: xEu
3+Wherein, Ca
1-x-yLu
yMoO
4Be matrix, Eu
3+Be dopant ion; The span of x is that the span of 0.1～0.2, y is 0.2～0.6.
Among the preparation method of above-mentioned europium doping molybdic acid lutetium calcium light-emitting film:
CaO in described step S1, Lu
2O
3, Eu
2O
3And MoO
3When the mass percent of raw material is respectively 15.8%, 26.8%, 8.9% and 48.5%; Correspondingly, among the step S4, the value of x is that the value of 0.15, y is 0.4;
Among the above-mentioned steps S1, the sintering temperature of preferred described preparation of target materials is 1250 ℃;
Among the above-mentioned steps S2, the vacuum tightness of preferred described vacuum cavity is arranged on 5.0 * 10
-4Pa;
Among the above-mentioned steps S3, preferred described basic target spacing is 60mm; Described magnetron sputtering operating pressure is 2.0Pa; The flow of described argon gas working gas is 25sccm; Described underlayer temperature is 500 ℃;
Among the above-mentioned steps S4, the annealing temperature during preferred described vacuum annealing is processed is 600 ℃, and annealing time is 2h.
Another purpose of the present invention is to provide a kind of organic electroluminescence device, and its luminescent layer is europium doping molybdic acid lutetium calcium light-emitting film, and the chemical general formula of this light-emitting film is Ca
1-x-yLu
yMoO
4: xEu
3+Wherein, Ca
1-x-yLu
yMoO
4Be matrix, Eu
3+Be dopant ion, the span of x is that the span of 0.1～0.2, y is 0.2～0.6; Preferably, the value of x is that the value of 0.15, y is 0.4.。
Europium doping molybdic acid lutetium calcium light-emitting film of the present invention adopts magnetron sputtering equipment to prepare, and in the electroluminescence spectrum of this light-emitting film (EL), its emitting red light peak is mainly by 614nm's
5D
0→
7F
2Electric dipole transition and 590nm's
5D
0→
7F
1Magnetic dipole transition forms.
Description of drawings
Fig. 1 is preparation technology's schema of europium doping molybdic acid lutetium calcium light-emitting film of the present invention;
Fig. 2 is the structural representation of organic electroluminescence device of the present invention;
Fig. 3 is the XRD figure of the europium doping molybdic acid lutetium calcium light-emitting film that makes of embodiment 1;
Fig. 4 is the electroluminescent spectrum of the europium doping molybdic acid lutetium calcium light-emitting film that obtains of embodiment 1.
Embodiment
The invention provides europium doping molybdic acid lutetium calcium light-emitting film, its chemical general formula is Ca
1-x-yLu
yMoO
4: xEu
3+Wherein, Ca
1-x-yLu
yMoO
4Be matrix, Eu
3+Be dopant ion, the span of x is that the span of 0.1～0.2, y is 0.2～0.6; Preferably, the value of x is that the value of 0.15, y is 0.4.
Europium doping molybdic acid lutetium calcium light-emitting film (Ca of the present invention
1-x-yLu
yMoO
4: xEu
3+), adopt magnetron sputtering equipment to prepare, in the electroluminescence spectrum of this light-emitting film (EL), its emitting red light peak is mainly by 614nm's
5D
0→
7F
2Electric dipole transition and 590nm's
5D
0→
7F
1Magnetic dipole transition forms.
The preparation method of above-mentioned europium doping molybdic acid lutetium calcium light-emitting film, as shown in Figure 1, its step of preparation process is as follows:
Step S1 by mass percentage, takes by weighing respectively 14～17.6% CaO, 13.4～40.2% Lu
2O
3, 5.9～11.8% Eu
2O
3And the MoO of surplus
3Raw material, and after even through ground and mixed, at 900～1300 ℃ of lower sintering, make target;
Step S2 packs the target that obtains among the step S1 and substrate in the vacuum cavity of magnetic-controlled sputtering coating equipment into, and the vacuum tightness of vacuum cavity is arranged on 1.0 * 10
-3Pa～1.0 * 10
-5Between the Pa;
Step S3, adjustment magnetron sputtering plating processing parameter is: basic target spacing is 45～95mm, and magnetron sputtering operating pressure 0.2～4Pa, the flow 10～35sccm of argon gas working gas, underlayer temperature are 250 ℃～750 ℃; Then be filmed, obtain film sample;
Step S4 processes 1～3h with the film sample that step S3 obtains in 500～800 ℃ of lower vacuum annealings, and obtaining chemical general formula is Ca
1-x-yLu
yMoO
4: xEu
3+Wherein, Ca
1-x-yLu
yMoO
4Be matrix, Eu
3+Be dopant ion, the span of x is that the span of 0.1～0.2, y is 0.2～0.6.
Among the preparation method of above-mentioned europium doping molybdic acid lutetium calcium light-emitting film:
CaO in described step S1, Lu
2O
3, Eu
2O
3And MoO
3When the mass percent of raw material is respectively 15.8%, 26.8%, 8.9% and 48.5%; Correspondingly, among the step S4, the value of x is that the value of 0.15, y is 0.4;
Among the above-mentioned steps S1, the sintering temperature of preferred described preparation of target materials is 1250 ℃;
Among the above-mentioned steps S2, the vacuum tightness of preferred described vacuum cavity is arranged on 5.0 * 10
-4Pa;
Among the above-mentioned steps S3, preferred described basic target spacing is 60mm; Described magnetron sputtering operating pressure is 2.0Pa; The flow of described argon gas working gas is 25sccm; Described underlayer temperature is 500 ℃;
Among the above-mentioned steps S4, the annealing temperature during preferred described vacuum annealing is processed is 600 ℃, and annealing time is 2h, and vacuum tightness is 0.01Pa.
Adopt above-mentioned technique to prepare europium doping molybdic acid lutetium calcium light-emitting film (Ca
1-x-yLu
yMoO
4: xEu
3+), its technical maturity, simple to operate is suitable for suitability for industrialized production.
The present invention also provides a kind of organic electroluminescence device, and the luminescent layer of this organic electroluminescence device adopts above-mentioned europium doping molybdic acid lutetium calcium light-emitting film, and the chemical general formula of this molybdic acid lutetium calcium light-emitting film is Ca
1-x-yLu
yMoO
4: xEu
3+Wherein, Ca
1-x-yLu
yMoO
4Be matrix, Eu
3+Be dopant ion, the span of x is that the span of 0.1～0.2, y is 0.2～0.6; Preferably, the value of x is that the value of 0.15, y is 0.4.
As shown in Figure 2, the stepped construction of this organic electroluminescence device is: substrate 1/ conductive anode layer 2/ luminescent layer 3/ cathode layer 4; Wherein, substrate 1 adopts glass, and conductive anode layer 2 adopts ITO, and two kinds are combined, referred to as ito glass; Ito glass can obtain by buying, and also can make by the method for magnetron sputtering; 3 of luminescent layers are surperficial at the ITO layer by the magnetron sputtering technique preparation; Cathode layer 4 adopts the Ag layer, by the surface of evaporation process preparation at luminescent layer.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
1, according to mass percent, take by weighing powder: CaO is 15.8%, Lu
2O
3Be 26.8%, Eu
2O
3Be 8.9% and MoO
3Be 48.5%; After these powders were even through ground and mixed, at 1250 ℃ of lower sintering, naturally cooling obtained the target sample, and it is that 50mm, thickness are the target of 2mm that the target sample is cut into diameter;
2, target is packed in the vacuum cavity of magnetic-controlled sputtering coating equipment;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass substrate, and to it, put into the vacuum cavity of magnetic-controlled sputtering coating equipment after complete; Wherein, the basic target spacing setting of target and glass is 60mm;
4, with mechanical pump and molecular pump the vacuum tightness of the vacuum cavity of magnetic-controlled sputtering coating equipment is extracted into 5.0 * 10
-4Pa;
5, adjust the magnetron sputtering plating processing parameter: argon gas working gas flow is 25sccm; The magnetron sputtering operating pressure is 2.0Pa; Underlayer temperature is 500 ℃; Then be filmed the film sample that obtains;
6, film sample is annealed in 0.01Pa vacuum oven 2h, annealing temperature is 600 ℃, obtains europium doping molybdic acid lutetium calcium light-emitting film, i.e. Ca
0.45Lu
0.4MoO
4: 0.15Eu
3+
Fig. 3 is the XRD figure of the europium doping molybdic acid lutetium calcium light-emitting film that makes of embodiment 1; Contrast PDF card, the diffraction peak among Fig. 3 is the peak crystallization of molybdic acid lutetium calcium matrix, the relevant peak of europium doped element do not occur, illustrates that doped element is the lattice that has entered matrix.
Fig. 4 is electroluminescent spectrum (EL) figure of the europium doping molybdic acid lutetium calcium light-emitting film that obtains of embodiment 1; As shown in Figure 4, the emitting red light peak is mainly by 614nm's
5D
0→
7F
2Electric dipole transition and 590nm's
5D
0→
7F
1Magnetic dipole transition forms.
Embodiment 2
1,, according to mass percent, take by weighing powder: CaO is 14%, Lu
2O
3Be 40.2%, Eu
2O
3Be 5.9% and MoO
3Be 39.9%; After these powders were even through ground and mixed, at 900 ℃ of lower sintering, naturally cooling obtained the target sample, and it is that 50mm, thickness are the target of 2mm that the target sample is cut into diameter;
2, target is packed in the vacuum cavity of magnetic-controlled sputtering coating equipment;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass, and to it, put into the vacuum cavity of magnetic-controlled sputtering coating equipment after complete; Wherein, the basic target spacing setting of target and glass is 45mm;
4, with mechanical pump and molecular pump the vacuum tightness of the vacuum cavity of magnetic-controlled sputtering coating equipment is extracted into 1.0 * 10
-3Pa;
5, adjust the magnetron sputtering plating processing parameter: argon gas working gas flow is 10sccm; The magnetron sputtering operating pressure is 4Pa; Underlayer temperature is 250 ℃; Then be filmed the film sample that obtains;
6, film sample is annealed in 0.01Pa vacuum oven 1h, annealing temperature is 500 ℃, obtains europium doping molybdic acid lutetium calcium light-emitting film, i.e. Ca
0.3Lu
0.6MoO
4: 0.1Eu
3+
Embodiment 3
1, according to mass percent, take by weighing powder: CaO is 17.6%, Lu
2O
3Be 13.4%, Eu
2O
3Be 11.8% and MoO
3Be 57.2%; After these powders were even through ground and mixed, at 1300 ℃ of lower sintering, naturally cooling obtained the target sample, and it is that 50mm, thickness are the target of 2mm that the target sample is cut into diameter;
2, target is packed in the vacuum cavity of magnetic-controlled sputtering coating equipment;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning band glass substrate, and to it, put into the vacuum cavity of magnetic-controlled sputtering coating equipment after complete; Wherein, the basic target spacing setting of target and glass is 95mm;
4, with mechanical pump and molecular pump the vacuum tightness of the vacuum cavity of magnetic-controlled sputtering coating equipment is extracted into 1.0 * 10
-5Pa;
5, adjust the magnetron sputtering plating processing parameter: argon gas working gas flow is 35sccm; The magnetron sputtering operating pressure is 0.2Pa; Underlayer temperature is 750 ℃; Then be filmed the film sample that obtains;
6, film sample is annealed in 0.01Pa vacuum oven 3h, annealing temperature is 800 ℃, obtains europium doping molybdic acid lutetium calcium light-emitting film, i.e. Ca
0.6Lu
0.2MoO
4: 0.2Eu
3+
Embodiment 4
Among the embodiment 4, a kind of preparation of electroluminescent device makes light-emitting film as the luminescent layer material with embodiment 1; Wherein, the substrate of this electroluminescent device is glass, and anode layer is ITO (tin indium oxide), plays electric action, and both are combined, and are called ito glass, can buy acquisition.
1, according to mass percent, take by weighing powder: CaO is 15.8%, Lu
2O
3Be 26.8%, Eu
2O
3Be 8.9% and MoO
3Be 48.5%; After these powders were even through ground and mixed, at 1250 ℃ of lower sintering, naturally cooling obtained the target sample, and it is that 50mm, thickness are the target of 2mm that the target sample is cut into diameter;
2, target is packed in the vacuum cavity of magnetic-controlled sputtering coating equipment;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning ito glass, and to it, put into the vacuum cavity of magnetic-controlled sputtering coating equipment after complete; Wherein, the basic target spacing setting of target and ito glass is 60mm;
4, with mechanical pump and molecular pump the vacuum tightness of the vacuum cavity of magnetic-controlled sputtering coating equipment is extracted into 5.0 * 10
-4Pa;
5, adjust the magnetron sputtering plating processing parameter: argon gas working gas flow is 25sccm; The magnetron sputtering operating pressure is 2.0Pa; Underlayer temperature is 500 ℃; Then be filmed the film sample that obtains;
6, film sample is annealed in 0.01Pa vacuum oven 2h, annealing temperature is 700 ℃, obtains europium doping molybdic acid lutetium calcium light-emitting film, i.e. Ca
1-x-yLu
yMoO
4: xEu
3+
7, adopt evaporation coating technique, the light-emitting film surface evaporation Ag layer in step 6 as cathode layer, makes organic electroluminescence device.
Should be understood that above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, scope of patent protection of the present invention should be as the criterion with claims.
Claims (10)
1. an europium doping molybdic acid lutetium calcium light-emitting film is characterized in that, the chemical general formula of this europium doping molybdic acid lutetium calcium light-emitting film is Ca
1-x-yLu
yMoO
4: xEu
3+Wherein, Ca
1-x-yLu
yMoO
4Be matrix, Eu
3+Be dopant ion, the span of x is that the span of 0.1～0.2, y is 0.2～0.6.
2. europium doping molybdic acid lutetium calcium light-emitting film according to claim 1 is characterized in that the value of x is that the value of 0.15, y is 0.4.
3. the preparation method of an europium doping molybdic acid lutetium calcium light-emitting film is characterized in that, comprises the steps:
Step S1 by mass percentage, takes by weighing respectively 14～17.6% CaO, 13.4～40.2% Lu
2O
3, 5.9～11.8% Eu
2O
3And the MoO of surplus
3Raw material, and after even through ground and mixed, at 900～1300 ℃ of lower sintering, make target;
Step S2 packs the target that obtains among the step S1 and substrate in the vacuum cavity of magnetic-controlled sputtering coating equipment into, and the vacuum tightness of vacuum cavity is arranged on 1.0 * 10
-3Pa～1.0 * 10
-5Between the Pa;
Step S3, adjustment magnetron sputtering plating processing parameter is: basic target spacing is 45～95mm, and magnetron sputtering operating pressure 0.2～4Pa, the flow 10～35sccm of argon gas working gas, underlayer temperature are 250 ℃～750 ℃; Then be filmed, obtain film sample;
Step S4 processes 1～3h with the film sample that step S3 obtains in 500～800 ℃ of lower vacuum annealings, and obtaining chemical general formula is Ca
1-x-yLu
yMoO
4: xEu
3+Wherein, Ca
1-x-yLu
yMoO
4Be matrix, Eu
3+Be dopant ion, the span of x is that the span of 0.1～0.2, y is 0.2～0.6.
4. the preparation method of europium doping molybdic acid lutetium calcium light-emitting film according to claim 3 is characterized in that, among the described step S1, and CaO, Lu
2O
3, Eu
2O
3And MoO
3When the mass percent of raw material is respectively 15.8%, 26.8%, 8.9% and 48.5%; Correspondingly, among the step S4, the value of x is that the value of 0.15, y is 0.4.
5. according to claim 3 or the preparation method of 4 described europium doping molybdic acid lutetium calcium light-emitting films, it is characterized in that among the described step S1, the sintering temperature of described preparation of target materials is 1250 ℃.
6. the preparation method of europium doping molybdic acid lutetium calcium light-emitting film according to claim 3 is characterized in that among the described step S2, the vacuum tightness of described vacuum cavity is arranged on 5.0 * 10
-4Pa.
7. the Preparation Method of europium doping molybdic acid lutetium calcium light-emitting film processed according to claim 3 is characterized in that, among the described step S3, described basic target spacing is 60mm; Described magnetron sputtering operating pressure is 2.0Pa; The flow of described argon gas working gas is 25sccm; Described underlayer temperature is 500 ℃.
8. the preparation method of europium doping molybdic acid lutetium calcium light-emitting film according to claim 3 is characterized in that, among the described step S4, the annealing temperature during described vacuum annealing is processed is 600 ℃, and annealing time is 2h.
9. an organic electroluminescence device is characterized in that, the luminescent layer of this organic electroluminescence device is europium doping molybdic acid lutetium calcium light-emitting film, and the chemical general formula of this europium doping molybdic acid lutetium calcium light-emitting film is Ca
1-x-yLu
yMoO
4: xEu
3+Wherein, Ca
1-x-yLu
yMoO
4Be matrix, Eu
3+Be dopant ion, the span of x is that the span of 0.1～0.2, y is 0.2～0.6.
10. organic electroluminescence device according to claim 9 is characterized in that, the value of x is that the value of 0.15, y is 0.4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110320324.XA CN103059854B (en) | 2011-10-19 | 2011-10-19 | Europium-doped calcium lutetium molybdate luminescent film, preparation method thereof, and organic electroluminescent device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110320324.XA CN103059854B (en) | 2011-10-19 | 2011-10-19 | Europium-doped calcium lutetium molybdate luminescent film, preparation method thereof, and organic electroluminescent device |
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| Publication Number | Publication Date |
|---|---|
| CN103059854A true CN103059854A (en) | 2013-04-24 |
| CN103059854B CN103059854B (en) | 2014-07-30 |
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| CN107522229A (en) * | 2017-07-24 | 2017-12-29 | 桂林理工大学 | One kind (Y1‑xLnx)2(MoO4)3The direct preparation method of film |
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| CN107522229B (en) * | 2017-07-24 | 2019-10-11 | 桂林理工大学 | One kind (Y1-xLnx)2(MoO4)3The direct preparation method of film |
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