CN102863952B - 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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- CN102863952B CN102863952B CN201110191521.6A CN201110191521A CN102863952B CN 102863952 B CN102863952 B CN 102863952B CN 201110191521 A CN201110191521 A CN 201110191521A CN 102863952 B CN102863952 B CN 102863952B
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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), due to its active illuminating, total solids, the advantage such as shock-resistant, reaction is fast, visual angle is large, Applicable temperature is wide, operation is simple, has caused and paid close attention to widely, and development rapidly.At present, research colour and extremely panchromatic TFELD, 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, have not yet to see report.
[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+, wherein 0.0008≤x≤0.0157,0.0007≤y≤0.0297.
In a preferred embodiment, x is that 0.0039, y is 0.0097.
A preparation method for the dysprosium co-doped calcium sulfate luminescent material of europium, comprises the following steps: step 1, according to CaSO
4: xEu
3+, yDy
3+the stoichiometric ratio of each element takes 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 mixing sintering at 900 DEG C～1300 DEG C is obtained to the dysprosium co-doped calcium sulfate luminescent material of described europium for 0.5 hour～5 hours.
In a preferred embodiment, x is that 0.0039, y is 0.0097.
In a preferred embodiment, in step 2 by the powder mixing sintering 3 hours at 1250 DEG C.
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+, wherein CaSO
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.
A preparation method for the dysprosium co-doped calcium sulfate light-emitting film of europium, comprises the following steps: step 1, according to CaSO
4: xEu
3+, yDy
3+the stoichiometric ratio of each element takes CaSO
4, Eu
2o
3and Dy
2o
3powder also mixes sintering at 900 DEG C～1300 DEG C and within 0.5 hour～5 hours, makes target, wherein 0.0008≤x≤0.0157,0.0007≤y≤0.0297; Step 2, the target obtaining in step 1 and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, 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: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C; Then be filmed, obtain film sample; Step 4, by the film sample obtaining in step 3 at 500 DEG C～800 DEG C vacuum annealing process 1h～3h, obtain the dysprosium co-doped calcium sulfate light-emitting film of described europium.
In a preferred embodiment, in step 1, x is that 0.0039, y is 0.0097; In step 2, vacuum tightness is 5.0 × 10
-4pa; In step 3, base target spacing is 60mm, magnetron sputtering operating pressure 2Pa, and working gas is argon gas, and the flow of working gas is 25sccm, and underlayer temperature is 500 DEG C; In step 4,2h is processed in film sample vacuum annealing at 600 DEG C.
A kind of membrane electro luminescent device, this membrane electro luminescent device comprises the substrate, anode layer, luminescent layer and the cathode layer that stack 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+, wherein 0.0008≤x≤0.0157,0.0007≤y≤0.0297.
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, there is very strong glow peak at 520nm and 610nm wavelength zone, can be applied in thin-film electroluminescent displays.
[brief description of the 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 prepared of embodiment 1;
Fig. 3 is the XRD figure of the dysprosium co-doped calcium sulfate light-emitting film of europium prepared of embodiment 1.
[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 europium of one embodiment, its chemical formula is CaSO
4: xEu
3+, yDy
3+, wherein 0.0008≤x≤0.0157,0.0007≤y≤0.0297, 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, there is very strong glow peak at 520nm and 610nm wavelength zone, can be applied in thin-film electroluminescent displays.
The preparation method of the dysprosium co-doped calcium sulfate luminescent material of above-mentioned europium, comprises the following steps:
Step S11, according to CaSO
4: xEu
3+, yDy
3+the stoichiometric ratio of each element takes 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 and in this step, also can take CaSO
4, Eu
2o
3and Dy
2o
3powder also mixes, wherein Eu
2o
3quality percentage composition be 0.1%～2%, Dy
2o
3quality percentage composition be 0.1%～4%, surplus is CaSO
4.Preferably, Eu
2o
3quality percentage composition be 0.5%, Dy
2o
3quality percentage composition be 1.3%.
Step S12, by mix equal powder sintering at 900 DEG C～1300 DEG C within 0.5 hour～5 hours, can obtain target product.
In this step, preferably sintering 3 hours at 1250 DEG C.
The dysprosium co-doped calcium sulfate light-emitting film of 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+, wherein CaSO
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, comprises the following steps:
Step S21, according to CaSO
4: xEu
3+, yDy
3+the stoichiometric ratio of each element takes CaSO
4, Eu
2o
3and Dy
2o
3powder also mixes sintering at 900 DEG C～1300 DEG C and within 0.5 hour～5 hours, makes target, 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 and in this step, also can take CaSO
4, Eu
2o
3and Dy
2o
3powder also mixes, wherein Eu
2o
3quality percentage composition be 0.1%～2%, Dy
2o
3quality percentage composition be 0.1%～4%, surplus is CaSO
4.Preferably, Eu
2o
3quality percentage composition be 0.5%, Dy
2o
3quality percentage composition be 1.3%.
Step S22, the target obtaining in step S21 and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, 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: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C; Then be filmed, obtain film sample.
In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 2Pa, and working gas is argon gas, and the flow of working gas is 25sccm, and underlayer temperature is 500 DEG C.
Step S24, by the film sample obtaining in step S23 at 500 DEG C～800 DEG C vacuum annealing process 1h～3h, obtaining chemical general formula is CaSO
4: xEu
3+, yDy
3+the dysprosium co-doped calcium sulfate light-emitting film of europium, wherein CaSO
4be matrix, Eu and Dy element are active elements, 0.0008≤x≤0.0157,0.0007≤y≤0.0297.
In this step, preferred, 2h is processed in film sample vacuum annealing at 600 DEG C.
Refer to Fig. 1, the thin-film electroluminescence (TFEL) device 100 of one embodiment, this membrane electro luminescent device 100 comprises the substrate 1, anode layer 2, luminescent layer 3 and the cathode layer 4 that stack 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+, wherein 0.0008≤x≤0.0157,0.0007≤y≤0.0297.
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, in the electroluminescence spectrum (EL) of film, having very strong glow peak at 520nm and 610nm wavelength zone, can be applied in thin-film electroluminescent displays.
Be specific embodiment below.
Embodiment 1
Selecting purity is 99.99% powder, the Eu that is 0.5% by quality percentage composition
2o
3, the Dy that quality percentage composition is 1.3%
2o
3with the quality percentage composition CaSO that is 98.2%
4, after even mixing, at 1250 DEG C, 3 hours one-tenth diameters of sintering are 50mm, the ceramic target that thickness is 2mm, and target is packed in 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 to oxygen plasma treatment, putting into vacuum cavity.The distance of target and substrate is set as to 60mm.The vacuum tightness of cavity is extracted into 5.0 × 10 with mechanical pump and molecular pump
-4pa, the working gas flow of argon gas is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C.The sample the obtaining 2h that anneals in 0.01Pa vacuum oven, annealing temperature is 600 DEG C.Then evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula of the dysprosium co-doped calcium sulfate light-emitting film of europium obtaining in the present embodiment is CaSO
4: 0.0039Eu
3+, 0.0097Dy
3+, wherein CaSO
4be matrix, Eu and Dy element are active elements.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the dysprosium co-doped calcium sulfate light-emitting film of the europium obtaining.As seen from Figure 2, in electroluminescence spectrum, there is very strong glow peak at 520nm and 610nm wavelength zone, can be applied in thin-film electroluminescent displays.
Refer to Fig. 3, Fig. 3 is the XRD curve of the dysprosium co-doped calcium sulfate light-emitting film of europium prepared of embodiment 1, test comparison standard P DF card.As can be seen from Figure 3, major part is the peak crystallization of calcium sulfate, does not occur the diffraction peak of doped element and other impurity.Europium ion and dysprosium ion Substitute For Partial calcium ion enter calcium sulfate lattice, do not change the original crystalline structure of calcium sulfate.
Embodiment 2
Selecting purity is 99.99% powder, the Eu that is 0.1% by quality percentage composition
2o
3, the Dy that quality percentage composition is 4%
2o
3with the quality percentage composition CaSO that is 95.9%
4, after even mixing, at 900 DEG C, within 5 hours, to make diameter be 50mm to sintering, the ceramic target that thickness is 2mm, and target is packed in 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 to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-3pa, the working gas flow of argon gas is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 DEG C.The sample the obtaining 1h that anneals in 0.01Pa vacuum oven, annealing temperature is 500 DEG C.Then evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula of the dysprosium co-doped calcium sulfate light-emitting film of europium obtaining in the present embodiment is CaSO
4: 0.0008Eu
3+, 0.0297Dy
3+, wherein CaSO
4be matrix, Eu and Dy element are active elements.
Embodiment 3
Selecting purity is 99.99% powder, the Eu that is 2% by quality percentage composition
2o
3, the Dy that quality percentage composition is 0.1%
2o
3with the quality percentage composition CaSO that is 97.9%
4, after even mixing, at 1300 DEG C, within 0.5 hour, to make diameter be 50mm to sintering, the ceramic target that thickness is 2mm, and target is packed in 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 to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 95mm.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-5pa, the working gas flow of argon gas is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C.The sample the obtaining 3h that anneals in 0.01Pa vacuum oven, annealing temperature is 800 DEG C.Then evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula of the dysprosium co-doped calcium sulfate light-emitting film of europium obtaining in the present embodiment is CaSO
4: 0.0157Eu
3+, 0.0007Dy
3+, wherein CaSO
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 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 (6)
1. the dysprosium co-doped calcium sulfate luminescent material of europium, is characterized in that: its chemical formula is CaSO
4: xEu
3+, yDy
3+, wherein x is that 0.0039, y is 0.0097.
2. a preparation method for the dysprosium co-doped calcium sulfate luminescent material of europium, is characterized in that, comprises the following steps:
Step 1, according to CaSO
4: xEu
3+, yDy
3+the stoichiometric ratio of each element takes CaSO
4, Eu
2o
3and Dy
2o
3powder also mixes, and wherein x is that 0.0039, y is 0.0097;
Step 2, the powder mixing sintering at 1250 DEG C is obtained to the dysprosium co-doped calcium sulfate luminescent material of described europium for 3 hours.
3. 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+, wherein CaSO
4be matrix, Eu and Dy element are active elements, and x is that 0.0039, y is 0.0097.
4. a preparation method for the dysprosium co-doped calcium sulfate light-emitting film of europium, is characterized in that, comprises the following steps:
Step 1, according to CaSO
4: xEu
3+, yDy
3+the stoichiometric ratio of each element takes CaSO
4, Eu
2o
3and Dy
2o
3powder also mixes sintering at 900 DEG C～1300 DEG C and within 0.5 hour～5 hours, makes target, and wherein x is that 0.0039, y is 0.0097;
Step 2, the target obtaining in step 1 and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, 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: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C; Then be filmed, obtain film sample;
Step 4, by the film sample obtaining in step 3 at 500 DEG C～800 DEG C vacuum annealing process 1h～3h, obtain the dysprosium co-doped calcium sulfate light-emitting film of described europium.
5. the preparation method of the dysprosium co-doped calcium sulfate light-emitting film of europium according to claim 4, is characterized in that, in step 1, x is that 0.0039, y is 0.0097; In step 2, vacuum tightness is 5.0 × 10
-4pa; In step 3, base target spacing is 60mm, magnetron sputtering operating pressure 2Pa, and working gas is argon gas, and the flow of working gas is 25sccm, and underlayer temperature is 500 DEG C; In step 4,2h is processed in film sample vacuum annealing at 600 DEG C.
6. a membrane electro luminescent device, this membrane electro luminescent device comprises the substrate, anode layer, luminescent layer and the cathode layer that stack 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+, wherein x is that 0.0039, y is 0.0097.
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|---|---|---|---|
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Non-Patent Citations (4)
| Title |
|---|
| Lakshmanan等.Photoluminescence and thermostimulated luminescence processes in rare-earth-doped CaSO4 phosphors.《Progress in Materials Science》.1999,第44卷(第1期),第129页. |
| Photoluminescence and thermostimulated luminescence processes in rare-earth-doped CaSO4 phosphors;Lakshmanan等;《Progress in Materials Science》;19991231;第44卷(第1期);第129页 * |
| 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)》.2003 |
| 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)》.2003,第32卷(第2期),51-54页. * |
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