CN102952545A - Europium-doped strontium vanadate luminescent film, preparation method and organic electroluminescent device - Google Patents
Europium-doped strontium vanadate luminescent film, preparation method and organic electroluminescent device Download PDFInfo
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- CN102952545A CN102952545A CN2011102466483A CN201110246648A CN102952545A CN 102952545 A CN102952545 A CN 102952545A CN 2011102466483 A CN2011102466483 A CN 2011102466483A CN 201110246648 A CN201110246648 A CN 201110246648A CN 102952545 A CN102952545 A CN 102952545A
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Abstract
The invention belongs to the field of photoelectric luminescent films, and discloses an europium-doped strontium vanadate luminescent film, a preparation method thereof, and an organic electroluminescent device; the general chemical formula of the luminescent film is Sr3-x(VO4)2:xEu3+, wherein Sr3-x(VO4)2 is a matrix, and Eu is the doping element; the value range of x is 0.005-0.015. According to the invention, the europium-doped strontium vanadate luminescent film is prepared by magnetron sputtering equipment, has a very strong luminescent band in a 6520-nm blue light zone, and has a very strong red luminescent peak at a 610-nm position.
Description
Technical field
The present invention relates to photo-electroluminescence film field, relate in particular to a kind of europium doping vanadic acid strontium light-emitting film and preparation method thereof.The invention still further relates to a kind of this europium doping vanadic acid strontium 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, research is colored to be reached to panchromatic TFELD, and the luminous material of exploitation multiband is the developing direction of this problem.
Europkium-activated vanadic acid yttrium phosphor powder is a kind of good red fluorescence material, has been widely used in high voltage mercury lamp, DPD demonstration etc. and has produced.In line with the use theory that reduces rare earth element, vanadic acid barium BaVO
4, vanadic acid strontium SrVO
4The fluorescence of class also is the active material of recently studying, but utilizes at present adulterated vanadate to be prepared into electroluminescent film, still rarely seen report.
Summary of the invention
The object of the invention be to provide a kind of take the vanadic acid strontium as matrix, the europium element is the europium doping vanadic acid strontium light-emitting film of main luminescence center.
Europium doping vanadic acid strontium light-emitting film of the present invention, its chemical general formula is Sr
3(VO
4)
2: xEu
3+Wherein, Sr
3-x(VO
4)
2Be matrix, Eu (europium) is doped element; The span of x is 0.005～0.015, x preferred 0.01.
Another goal of the invention of the present invention is to provide the preparation method of above-mentioned europium doping vanadic acid strontium light-emitting film, and its preparation technology is as follows:
The preparation of step S1, target: according to mass percent 55～70%, 0.008～0.023%, 29.992～44.977%, take by weighing respectively SrO, Eu
2O
3And V
2O
5Powder after the process ground and mixed is even, at 900～1300 ℃ of lower sintering, is made target;
Step S2, with pack into the vacuum cavity of magnetic-controlled sputtering coating equipment of the target among the step S1 and substrate, with mechanical pump and molecular pump the vacuum tightness of cavity is evacuated to 1.0 * 10
-3Pa～1.0 * 10
-5Pa, preferred vacuum tightness is 5.0 * 10
-4Pa;
Step S3, adjustment magnetron sputtering plating processing parameter are: basic target spacing is 45～95mm, preferred 60mm; Underlayer temperature is 250 ℃～750 ℃, preferred 500 ℃; Gas flow 10～the 35sccm of argon gas working gas, preferred 25sccm; Magnetron sputtering operating pressure 0.2～4Pa, preferred 2.0Pa; After processing parameter has been adjusted, then be filmed, obtain film sample;
Step S4, the film sample that step S3 is obtained place vacuum oven, (being 0.01Pa) anneal 1～3h under 500～800 ℃ (preferred 600 ℃), vacuum state (preferred 2h), and obtaining chemical general formula is Sr
3-x(VO
4)
2: xEu
3+Described europium doping vanadic acid strontium light-emitting film; Wherein, Sr
3-x(VO
4)
2Be matrix, Eu is doped element, and the span of x is 0.005～0.015.
In the above-mentioned preparation method, among the step S1, as SrO, Eu
2O
3And V
2O
5When the mass percent of powder was respectively 63%, 0.015% and 36.985%, correspondingly, among the step S4, the value of x was 0.01.
Another purpose of the present invention is to provide a kind of organic electroluminescence device, and this device is straticulate structure, and this straticulate structure is followed successively by substrate, anode layer, luminescent layer and cathode layer; Wherein, luminescent layer is that (chemical general formula of this light-emitting film is Sr to europium doping vanadic acid strontium light-emitting film
3-x(VO
4)
2: xEu
3+Wherein, Sr
3-x(VO
4)
2Be matrix, Eu is doped element, and the span of x is 0.005～0.015; X preferred 0.01); Substrate is glass, and anode layer is ITO, and cathode layer is the Ag layer, and the Ag layer adopts the evaporation process preparation at film surface.
The present invention adopts magnetron sputtering equipment, and preparation europium doping vanadic acid strontium light-emitting film obtains at the 520nm blue light region stronger luminous zone being arranged in the electroluminescent spectrum (EL) of film, and there is very strong emitting red light peak the 610nm position.。
Description of drawings
Fig. 1 is preparation technology's schema of europium doping vanadic acid strontium 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 vanadic acid strontium light-emitting film that makes of embodiment 1;
Fig. 4 is the electroluminescent spectrum that embodiment 1 obtains europium doping vanadic acid strontium light-emitting film.
Embodiment
A kind of europium doping vanadic acid strontium light-emitting film provided by the invention, it is Sr that this europium doping vanadic acid strontium light-emitting film comprises the film general formula
3-x(VO
4)
2: xEu
3+Wherein, Sr
3-x(VO
4)
2Be matrix, Eu is doped element; The span of x is 0.005～0.015, x preferred 0.01.
Above-mentioned europium doping vanadic acid strontium light-emitting film preparation method, as shown in Figure 1, its preparation technology is as follows:
The preparation of step S1, target: according to mass percent 55～70%, 0.008～0.023%, 29.992～44.977%, take by weighing respectively SrO, Eu
2O
3And V
2O
5Powder, after the process ground and mixed was even, at 900～1300 ℃ (preferred 1250 ℃) 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;
Step S2, with the vacuum cavity of the target among the step S1 and substrate (such as, the glass) magnetic-controlled sputtering coating equipment of packing into, with mechanical pump and molecular pump the vacuum tightness of cavity is evacuated to 1.0 * 10
-3Pa～1.0 * 10
-5Pa, preferred 5.0 * 10
-4Pa;
Step S3, adjustment magnetron sputtering plating processing parameter are: basic target spacing is 45～95mm, preferred 60mm; Underlayer temperature is 250 ℃～750 ℃, preferred 500 ℃; Gas flow 10～the 35sccm of argon gas working gas, preferred 25sccm; Magnetron sputtering operating pressure 0.2～4Pa, preferred 2.0Pa; After the processing parameter adjustment is complete, then be filmed, obtain film sample;
Step S4, the film sample that step S3 is obtained place vacuum oven, (being 0.01Pa) anneal 1～3h under 500～800 ℃ (preferred 600 ℃), vacuum state (preferred 2h), and obtaining chemical general formula is Sr
3-x(VO
4)
2: xEu
3+Described europium doping vanadic acid strontium light-emitting film; Wherein, Sr
3-x(VO
4)
2Be matrix, Eu is doped element, and the span of x is 0.005～0.015.
In the above-mentioned preparation method, among the step S1, as SrO, Eu
2O
3And V
2O
5When the mass percent of powder was respectively 63%, 0.015% and 36.985%, correspondingly, among the step S4, the value of x was 0.01.
The present invention also provides a kind of organic electroluminescence device, and as shown in Figure 2, this organic electroluminescence device comprises substrate 1, anode layer 2, luminescent layer 3 and the cathode layer 4 that stacks gradually; Wherein, substrate 1 is glass, and anode layer is the ITO layer, and both are combined and are ito glass, can buy acquisition; (chemical general formula of this light-emitting film is Sr to luminescent layer 3 for europium doping vanadic acid strontium light-emitting film layer
3-x(VO
4)
2: xEu
3+Wherein, Sr
3-x(VO
4)
2Be matrix, Eu is doped element, and the span of x is 0.005～0.015; X preferred 0.01), cathode layer 4 is the Ag layer, the Ag layer adopts the evaporation process preparation on europium doping vanadic acid strontium light-emitting film layer surface.
The present invention adopts magnetron sputtering equipment, and preparation europium doping vanadic acid strontium light-emitting film obtains at the 520nm blue light region stronger luminous zone being arranged in the electroluminescent spectrum (EL) of film, and there is very strong emitting red light peak the 610nm position.
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: SrO account for total amount 63%, Eu
2O
3Account for total amount 0.015%, V
2O
5Account for 36.985% of total amount; 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 vanadic acid strontium light-emitting film, i.e. Sr
2.99(VO
4)
2: 0.01Eu
3+
Fig. 3 is the XRD figure of the europium doping vanadic acid strontium light-emitting film that makes of embodiment 1; As can be seen from Figure 3, reference standard PDF card, diffraction peak is Sr
2.99(VO
4)
2The peak of matrix, the assorted peak that no dopant is relevant.
Fig. 4 is electroluminescent spectrum (EL) figure that embodiment 1 obtains europium doping vanadic acid strontium light-emitting film.As shown in Figure 4, obtain at the 520nm blue light region stronger luminous zone being arranged in the electroluminescent spectrum (EL) of film, there is very strong emitting red light peak the 610nm position.
Embodiment 2
1,, according to mass percent, take by weighing powder: SrO account for total amount 55%, Eu
2O
3Account for total amount 0.023%, V
2O
5Account for 44.977% of total amount; 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 vanadic acid strontium light-emitting film, i.e. Sr
2.985(VO
4)
2: 0.015Eu
3+
Embodiment 3
1, according to mass percent, take by weighing powder: SrO account for total amount 70%, Eu
2O
3Account for total amount 0.008%, V
2O
5Account for 22.992% of total amount; 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 vanadic acid strontium light-emitting film, i.e. Sr
2.995(VO
4)
2: 0.005Eu
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: SrO account for total amount 63%, Eu
2O
3Account for total amount 0.015%, V
2O
5Account for 36.985% of total amount; 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 vanadic acid strontium light-emitting film, i.e. Sr
2.99(VO
4)
2: 0.01Eu
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 vanadic acid strontium light-emitting film is characterized in that the chemical general formula of this light-emitting film is Sr
3-x(VO
4)
2: xEu
3+Wherein, Sr
3-x(VO
4)
2Be matrix, Eu is doped element, and the span of x is 0.005～0.015.
2. europium doping vanadic acid strontium light-emitting film according to claim 1 is characterized in that the value of x is 0.01.
3. the preparation method of an europium doping vanadic acid strontium light-emitting film is characterized in that, comprises the steps:
Step S1 according to mass percent 55～70%, 0.008～0.023%, 29.992～44.977%, takes by weighing respectively SrO, Eu
2O
3And V
2O
5Powder after the process ground and mixed is even, at 900～1300 ℃ of lower sintering, is made 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 Sr
3-x(VO
4)
2: xEu
3+Described europium doping vanadic acid strontium light-emitting film; Wherein, Sr
3-x(VO
4)
2Be matrix, Eu is doped element, and the span of x is 0.005～0.015.
4. the preparation method of europium doping vanadic acid strontium light-emitting film according to claim 3 is characterized in that, among the described step S1, as SrO, Eu
2O
3And V
2O
5When the mass percent of powder was respectively 63%, 0.015% and 36.985%, correspondingly, among the step S4, the value of x was 0.01.
5. according to claim 3 or the preparation method of 4 described europium doping vanadic acid strontium 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 vanadic acid strontium 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 vanadic acid strontium 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 vanadic acid strontium 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. organic electroluminescence device, this organic electroluminescence device is straticulate structure, and this straticulate structure is followed successively by substrate, anode layer, luminescent layer and cathode layer, it is characterized in that, described luminescent layer is europium doping vanadic acid strontium light-emitting film, and the chemical general formula of this light-emitting film is Sr
3-x(VO
4)
2: xEu
3+Wherein, Sr
3-x(VO
4)
2Be matrix, Eu is doped element, and the span of x is 0.005～0.015.
10. organic electroluminescence device according to claim 9 is characterized in that, the value of x is 0.01.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105154078A (en) * | 2015-10-09 | 2015-12-16 | 桂林理工大学 | Preparation method for fluorescent powder Sr3-3x/2(VO4)2:chi Eu<3+> |
| CN107871793A (en) * | 2016-09-27 | 2018-04-03 | 韩山师范学院 | Silica-based solar cell and its manufacture method |
| CN107868941A (en) * | 2016-09-27 | 2018-04-03 | 韩山师范学院 | The manufacture method of down-conversion luminescent material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105154078A (en) * | 2015-10-09 | 2015-12-16 | 桂林理工大学 | Preparation method for fluorescent powder Sr3-3x/2(VO4)2:chi Eu<3+> |
| CN107871793A (en) * | 2016-09-27 | 2018-04-03 | 韩山师范学院 | Silica-based solar cell and its manufacture method |
| CN107868941A (en) * | 2016-09-27 | 2018-04-03 | 韩山师范学院 | The manufacture method of down-conversion luminescent material |
| CN107868941B (en) * | 2016-09-27 | 2018-11-09 | 韩山师范学院 | The manufacturing method of down-conversion luminescent material |
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