CN102863952A - Europium-dysprosium codoped calcium sulfate luminescent material, preparation method and application thereof - Google Patents
Europium-dysprosium codoped calcium sulfate luminescent material, preparation method and application thereof Download PDFInfo
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- CN102863952A CN102863952A CN2011101915216A CN201110191521A CN102863952A CN 102863952 A CN102863952 A CN 102863952A CN 2011101915216 A CN2011101915216 A CN 2011101915216A CN 201110191521 A CN201110191521 A CN 201110191521A CN 102863952 A CN102863952 A CN 102863952A
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- dysprosium
- europium
- calcium sulfate
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Abstract
The invention provides a europium-dysprosium codoped calcium sulfate luminescent material. The chemical formula of the europium-dysprosium codoped calcium sulfate luminescent material is CaSO4:xEu3+, yDy3+, wherein x is more than or equal to 0.0008 and less than or equal to 0.0157, and y is more than or equal to 0.0007 and less than or equal to 0.0297. The electroluminescent spectrum (EL) of a luminescent film prepared by the europium-dysprosium codoped calcium sulfate luminescent material has a strong luminescent peak at the 520nm and 610nm wavelength areas and the luminescent film can be applied in a film electroluminescent display. The invention also provides a preparation method of the europium-dysprosium codoped calcium sulfate luminescent material, a europium-dysprosium codoped calcium sulfate luminescent film, a preparation method thereof and a film electroluminescent device.
Description
[technical field]
The present invention relates to the dysprosium co-doped calcium sulfate luminescent material of a kind of europium, its preparation method, the dysprosium co-doped calcium sulfate light-emitting film of europium, its preparation method and membrane electro luminescent device.
[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.But, can be applicable to the dysprosium co-doped calcium sulfate luminescent material of europium of thin-film electroluminescent displays, do not appear in the newspapers yet.
[summary of the invention]
Based on this, be necessary to provide a kind of membrane electro luminescent device that can be applicable to the dysprosium co-doped calcium sulfate luminescent material of europium, its preparation method, the dysprosium co-doped calcium sulfate light-emitting film of europium, its preparation method of membrane electro luminescent device and use the dysprosium co-doped calcium sulfate luminescent material of this europium.
The dysprosium co-doped calcium sulfate luminescent material of a kind of europium, its chemical formula is CaSO
4: xEu
3+, yDy
3+, 0.0008≤x≤0.0157,0.0007≤y≤0.0297 wherein.
In a preferred embodiment, x is that 0.0039, y is 0.0097.
The preparation method of the dysprosium co-doped calcium sulfate luminescent material of a kind of europium may further comprise the steps: step 1, according to CaSO
4: xEu
3+, yDy
3+The stoichiometric ratio of each element takes by weighing CaSO
4, Eu
2O
3And Dy
2O
3Powder also mixes, wherein 0.0008≤x≤0.0157,0.0007≤y≤0.0297; Step 2, the powder that mixes was namely obtained the dysprosium co-doped calcium sulfate luminescent material of described europium in 0.5 hour～5 hours at 900 ℃～1300 ℃ lower sintering.
In a preferred embodiment, x is that 0.0039, y is 0.0097.
In a preferred embodiment, in the step 2 with the powder that mixes 1250 ℃ of lower sintering 3 hours.
The dysprosium co-doped calcium sulfate light-emitting film of a kind of europium, the chemical general formula of the material of the dysprosium co-doped calcium sulfate light-emitting film of this europium is CaSO
4: xEu
3+, yDy
3+, CaSO wherein
4Be matrix, Eu and Dy element are active elements, 0.0008≤x≤0.0157,0.0007≤y≤0.0297.
In a preferred embodiment, x is that 0.0039, y is 0.0097.
The preparation method of the dysprosium co-doped calcium sulfate light-emitting film of a kind of europium may further comprise the steps: step 1, according to CaSO
4: xEu
3+, yDy
3+The stoichiometric ratio of each element takes by weighing CaSO
4, Eu
2O
3And Dy
2O
3Powder also mixes at 900 ℃～1300 ℃ lower sintering and made target, wherein 0.0008≤x≤0.0157,0.0007≤y≤0.0297 in 0.5 hour～5 hours; Step 2, with pack into the vacuum cavity of magnetic-controlled sputtering coating equipment of the target that obtains in the step 1 and substrate, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3Pa～1.0 * 10
-5Pa; Step 3, adjustment magnetron sputtering plating processing parameter are: basic target spacing is 45mm～95mm, and magnetron sputtering operating pressure 0.2Pa～4Pa, the flow of working gas are 10sccm～35sccm, and underlayer temperature is 250 ℃～750 ℃; Then be filmed, obtain film sample; Step 4, the film sample that obtains in the step 3 is processed 1h～3h in 500 ℃～800 ℃ lower vacuum annealings, obtain the dysprosium co-doped calcium sulfate light-emitting film of described europium.
In a preferred embodiment, x is that 0.0039, y is 0.0097 in the step 1; Vacuum tightness is 5.0 * 10 in the step 2
-4Pa; In the step 3, basic target spacing is 60mm, and magnetron sputtering operating pressure 2Pa, working gas are argon gas, and the flow of working gas is 25sccm, and underlayer temperature is 500 ℃; In the step 4, film sample is processed 2h in 600 ℃ of lower vacuum annealings.
A kind of membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer that stacks gradually, the material of described luminescent layer is the dysprosium co-doped calcium sulfate luminescent material of europium, and the chemical formula of the dysprosium co-doped calcium sulfate luminescent material of this europium is CaSO
4: xEu
3+, yDy
3+, 0.0008≤x≤0.0157,0.0007≤y≤0.0297 wherein.
The dysprosium co-doped calcium sulfate luminescent material of above-mentioned europium (CaSO
4: xEu
3+, yDy
3+) in the electroluminescent spectrum (EL) of the light-emitting film made, at 520nm and 610nm wavelength zone very strong glow peak being arranged, can be applied in the thin-film electroluminescent displays.
[description of drawings]
Fig. 1 is the structural representation of the membrane electro luminescent device of an embodiment;
Fig. 2 is the electroluminescent spectrogram of the dysprosium co-doped calcium sulfate light-emitting film of europium of embodiment 1 preparation;
Fig. 3 is the XRD figure of the dysprosium co-doped calcium sulfate light-emitting film of europium of embodiment 1 preparation.
[embodiment]
Below in conjunction with the drawings and specific embodiments the dysprosium co-doped calcium sulfate luminescent material of europium, its preparation method, the dysprosium co-doped calcium sulfate light-emitting film of europium, its preparation method and membrane electro luminescent device are further illustrated.
The dysprosium co-doped calcium sulfate luminescent material of the europium of one embodiment, its chemical formula is CaSO
4: xEu
3+, yDy
3+, 0.0008≤x≤0.0157,0.0007≤y≤0.0297 wherein, preferred, x is that 0.0039, y is 0.0097.
CaSO in the dysprosium co-doped calcium sulfate luminescent material of this europium
4Be matrix, Eu and Dy element are active elements.In the electroluminescent spectrum (EL) of the light-emitting film that the dysprosium co-doped calcium sulfate luminescent material of this europium is made, at 520nm and 610nm wavelength zone very strong glow peak is arranged, can be applied in the thin-film electroluminescent displays.
The preparation method of the dysprosium co-doped calcium sulfate luminescent material of above-mentioned europium may further comprise the steps:
Step S11, according to CaSO
4: xEu
3+, yDy
3+The stoichiometric ratio of each element takes by weighing CaSO
4, Eu
2O
3And Dy
2O
3Powder, wherein 0.0008≤x≤0.0157,0.0007≤y≤0.0297.
In this step, preferred, x is that 0.0039, y is 0.0097.
Be appreciated that in this step and also can take by weighing CaSO
4, Eu
2O
3And Dy
2O
3Powder also mixes, wherein Eu
2O
3The quality percentage composition be 0.1%～2%, Dy
2O
3The quality percentage composition be 0.1%～4%, surplus is CaSO
4Preferably, Eu
2O
3The quality percentage composition be 0.5%, Dy
2O
3The quality percentage composition be 1.3%.
Step S12, will mix equal powder and can obtain target product in 0.5 hour～5 hours at 900 ℃～1300 ℃ lower sintering.
In this step, preferably 1250 ℃ of lower sintering 3 hours.
The dysprosium co-doped calcium sulfate light-emitting film of the europium of one embodiment, the chemical general formula of the material of the dysprosium co-doped calcium sulfate light-emitting film of this europium is CaSO
4: xEu
3+, yDy
3+, CaSO wherein
4Be matrix, Eu and Dy element are active elements, 0.0008≤x≤0.0157,0.0007≤y≤0.0297.
Preferably, x is that 0.0039, y is 0.0097.
The preparation method of the dysprosium co-doped calcium sulfate light-emitting film of above-mentioned europium may further comprise the steps:
Step S21, according to CaSO
4: xEu
3+, yDy
3+The stoichiometric ratio of each element takes by weighing CaSO
4, Eu
2O
3And Dy
2O
3Powder also mixes at 900 ℃～1300 ℃ lower sintering and made target, wherein 0.0008≤x≤0.0157,0.0007≤y≤0.0297 in 0.5 hour～5 hours.
In this step, preferred, x is that 0.0039, y is 0.0097.
Be appreciated that in this step and also can take by weighing CaSO
4, Eu
2O
3And Dy
2O
3Powder also mixes, wherein Eu
2O
3The quality percentage composition be 0.1%～2%, Dy
2O
3The quality percentage composition be 0.1%～4%, surplus is CaSO
4Preferably, Eu
2O
3The quality percentage composition be 0.5%, Dy
2O
3The quality percentage composition be 1.3%.
Step S22, with pack into the vacuum cavity of magnetic-controlled sputtering coating equipment of the target that obtains among the step S21 and substrate, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3Pa～1.0 * 10
-5Pa.
In this step, preferred, vacuum tightness is 5 * 10
-4Pa.
Step S23, adjustment magnetron sputtering plating processing parameter are: basic target spacing is 45mm～95mm, and magnetron sputtering operating pressure 0.2Pa～4Pa, the flow of working gas are 10sccm～35sccm, and underlayer temperature is 250 ℃～750 ℃; Then be filmed, obtain film sample.
In this step, preferred basic target spacing is 60mm, and magnetron sputtering operating pressure 2Pa, working gas are argon gas, and the flow of working gas is 25sccm, and underlayer temperature is 500 ℃.
Step S24, the film sample that obtains among the step S23 is processed 1h～3h in 500 ℃～800 ℃ lower vacuum annealings, obtaining chemical general formula is CaSO
4: xEu
3+, yDy
3+The dysprosium co-doped calcium sulfate light-emitting film of europium, CaSO wherein
4Be matrix, Eu and Dy element are active elements, 0.0008≤x≤0.0157,0.0007≤y≤0.0297.
In this step, preferred, film sample is processed 2h 600 ℃ of lower vacuum annealings.
See also Fig. 1, the thin-film electroluminescence (TFEL) device 100 of one embodiment, this membrane electro luminescent device 100 comprises substrate 1, anode layer 2, luminescent layer 3 and the cathode layer 4 that stacks gradually, the material of described luminescent layer 3 is the dysprosium co-doped calcium sulfate luminescent material of europium, and the chemical formula of the dysprosium co-doped calcium sulfate luminescent material of this europium is CaSO
4: xEu
3+, yDy
3+, 0.0008≤x≤0.0157,0.0007≤y≤0.0297 wherein.
Adopt magnetron sputtering equipment, utilize the dysprosium co-doped calcium sulfate luminescent material of europium to prepare the dysprosium co-doped calcium sulfate light-emitting film of europium (CaSO
4: xEu
3+, yDy
3+), obtaining at 520nm and 610nm wavelength zone very strong glow peak being arranged in the electroluminescence spectrum (EL) of film, can be applied in the thin-film electroluminescent displays.
The below is specific embodiment.
Embodiment 1
Selecting purity is 99.99% powder, is 0.5% Eu with the quality percentage composition
2O
3, the quality percentage composition is 1.3% Dy
2O
3With the quality percentage composition be 98.2% CaSO
4, after evenly mixing, becoming diameter in 3 hours at 1250 ℃ of lower sintering is 50mm, thickness is the ceramic target of 2mm, and target is packed in the vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band tin indium oxide (ITO) and use it is carried out oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as 60mm.With mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 5.0 * 10
-4Pa, the working gas flow of argon gas is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 ℃.The sample that the obtains 2h that anneals in the 0.01Pa vacuum oven, annealing temperature is 600 ℃.Then evaporation one deck Ag on light-emitting film is as negative electrode.
The chemical general formula of the dysprosium co-doped calcium sulfate light-emitting film of the europium that obtains in the present embodiment is CaSO
4: 0.0039Eu
3+, 0.0097Dy
3+, CaSO wherein
4Be matrix, Eu and Dy element are active elements.
See also Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the dysprosium co-doped calcium sulfate light-emitting film of the europium that obtains.As seen from Figure 2, in the electroluminescence spectrum, at 520nm and 610nm wavelength zone very strong glow peak is arranged, can be applied in the thin-film electroluminescent displays.
See also Fig. 3, Fig. 3 is the XRD curve of the dysprosium co-doped calcium sulfate light-emitting film of europium of embodiment 1 preparation, test comparison standard P DF card.As can be seen from Figure 3, major part is the peak crystallization of calcium sulfate, the diffraction peak of doped element and other impurity do not occur.Europium ion and dysprosium ion Substitute For Partial calcium ion enter the calcium sulfate lattice, do not change the original crystalline structure of calcium sulfate.
Embodiment 2
Selecting purity is 99.99% powder, is 0.1% Eu with the quality percentage composition
2O
3, the quality percentage composition is 4% Dy
2O
3With the quality percentage composition be 95.9% CaSO
4, after evenly mixing, making diameter in 5 hours at 900 ℃ of lower sintering is 50mm, thickness is the ceramic target of 2mm, and target is packed in the vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as 45mm.With mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 1.0 * 10
-3Pa, the working gas flow of argon gas is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 ℃.The sample that the obtains 1h that anneals in the 0.01Pa vacuum oven, annealing temperature is 500 ℃.Then evaporation one deck Ag on light-emitting film is as negative electrode.
The chemical general formula of the dysprosium co-doped calcium sulfate light-emitting film of the europium that obtains in the present embodiment is CaSO
4: 0.0008Eu
3+, 0.0297Dy
3+, CaSO wherein
4Be matrix, Eu and Dy element are active elements.
Embodiment 3
Selecting purity is 99.99% powder, is 2% Eu with the quality percentage composition
2O
3, the quality percentage composition is 0.1% Dy
2O
3With the quality percentage composition be 97.9% CaSO
4, after evenly mixing, making diameter in 0.5 hour at 1300 ℃ of lower sintering is 50mm, thickness is the ceramic target of 2mm, and target is packed in the vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as 95mm.With mechanical pump and molecular pump the vacuum tightness of cavity is extracted into 1.0 * 10
-5Pa, the working gas flow of argon gas is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 ℃.The sample that the obtains 3h that anneals in the 0.01Pa vacuum oven, annealing temperature is 800 ℃.Then evaporation one deck Ag on light-emitting film is as negative electrode.
The chemical general formula of the dysprosium co-doped calcium sulfate light-emitting film of the europium that obtains in the present embodiment is CaSO
4: 0.0157Eu
3+, 0.0007Dy
3+, CaSO wherein
4Be matrix, Eu and Dy element are active elements.
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 claim of the present invention.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. dysprosium co-doped calcium sulfate luminescent material of europium, it is characterized in that: its chemical formula is CaSO
4: xEu
3+, yDy
3+, 0.0008≤x≤0.0157,0.0007≤y≤0.0297 wherein.
2. the dysprosium co-doped calcium sulfate luminescent material of europium according to claim 1 is characterized in that, x is that 0.0039, y is 0.0097.
3. the preparation method of the dysprosium co-doped calcium sulfate luminescent material of europium is characterized in that, may further comprise the steps:
Step 1, according to CaSO
4: xEu
3+, yDy
3+The stoichiometric ratio of each element takes by weighing CaSO
4, Eu
2O
3And Dy
2O
3Powder also mixes, wherein 0.0008≤x≤0.0157,0.0007≤y≤0.0297;
Step 2, the powder that mixes was namely obtained the dysprosium co-doped calcium sulfate luminescent material of described europium in 0.5 hour～5 hours at 900 ℃～1300 ℃ lower sintering.
4. the preparation method of the dysprosium co-doped calcium sulfate luminescent material of europium according to claim 3 is characterized in that, x is that 0.0039, y is 0.0097.
5. the preparation method of the dysprosium co-doped calcium sulfate luminescent material of europium according to claim 3 is characterized in that, in the step 2 with the powder that mixes 1250 ℃ of lower sintering 3 hours.
6. the dysprosium co-doped calcium sulfate light-emitting film of europium is characterized in that the chemical general formula of the material of the dysprosium co-doped calcium sulfate light-emitting film of this europium is CaSO
4: xEu
3+, yDy
3+, CaSO wherein
4Be matrix, Eu and Dy element are active elements, 0.0008≤x≤0.0157,0.0007≤y≤0.0297.
7. the dysprosium co-doped calcium sulfate light-emitting film of europium according to claim 6 is characterized in that, x is that 0.0039, y is 0.0097.
8. the preparation method of the dysprosium co-doped calcium sulfate light-emitting film of europium is characterized in that, may further comprise the steps:
Step 1, according to CaSO
4: xEu
3+, yDy
3+The stoichiometric ratio of each element takes by weighing CaSO
4, Eu
2O
3And Dy
2O
3Powder also mixes at 900 ℃～1300 ℃ lower sintering and made target, wherein 0.0008≤x≤0.0157,0.0007≤y≤0.0297 in 0.5 hour～5 hours;
Step 2, with pack into the vacuum cavity of magnetic-controlled sputtering coating equipment of the target that obtains in the step 1 and substrate, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3Pa～1.0 * 10
-5Pa;
Step 3, adjustment magnetron sputtering plating processing parameter are: basic target spacing is 45mm～95mm, and magnetron sputtering operating pressure 0.2Pa～4Pa, the flow of working gas are 10sccm～35sccm, and underlayer temperature is 250 ℃～750 ℃; Then be filmed, obtain film sample;
Step 4, the film sample that obtains in the step 3 is processed 1h～3h in 500 ℃～800 ℃ lower vacuum annealings, obtain the dysprosium co-doped calcium sulfate light-emitting film of described europium.
9. the preparation method of the dysprosium co-doped calcium sulfate light-emitting film of europium according to claim 8 is characterized in that, x is that 0.0039, y is 0.0097 in the step 1; Vacuum tightness is 5.0 * 10 in the step 2
-4Pa; In the step 3, basic target spacing is 60mm, and magnetron sputtering operating pressure 2Pa, working gas are argon gas, and the flow of working gas is 25sccm, and underlayer temperature is 500 ℃; In the step 4, film sample is processed 2h in 600 ℃ of lower vacuum annealings.
10. membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer that stacks gradually, it is characterized in that, the material of described luminescent layer is the dysprosium co-doped calcium sulfate luminescent material of europium, and the chemical formula of the dysprosium co-doped calcium sulfate luminescent material of this europium is CaSO
4: xEu
3+, yDy
3+, 0.0008≤x≤0.0157,0.0007≤y≤0.0297 wherein.
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113016080A (en) * | 2018-11-15 | 2021-06-22 | 株式会社日立高新技术 | Broadband light source device and biochemical analysis device |
-
2011
- 2011-07-08 CN CN201110191521.6A patent/CN102863952B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| LAKSHMANAN等: "Photoluminescence and thermostimulated luminescence processes in rare-earth-doped CaSO4 phosphors", 《PROGRESS IN MATERIALS SCIENCE》 * |
| 熊娟等: "Y3+ ,La3+对CaSO4:Eu2+发光性质的影响", 《上海师范大学学报(自然科学版)》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113016080A (en) * | 2018-11-15 | 2021-06-22 | 株式会社日立高新技术 | Broadband light source device and biochemical analysis device |
| CN113016080B (en) * | 2018-11-15 | 2024-04-16 | 株式会社日立高新技术 | Broadband light source device and biochemical analysis device |
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