CN103421509A - Cerium doped vanadium yttrium phosphate salt luminescent material and preparation method and application thereof - Google Patents
Cerium doped vanadium yttrium phosphate salt luminescent material and preparation method and application thereof Download PDFInfo
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- CN103421509A CN103421509A CN2012101512031A CN201210151203A CN103421509A CN 103421509 A CN103421509 A CN 103421509A CN 2012101512031 A CN2012101512031 A CN 2012101512031A CN 201210151203 A CN201210151203 A CN 201210151203A CN 103421509 A CN103421509 A CN 103421509A
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Abstract
A cerium doped vanadium yttrium phosphate salt luminescent material has a chemical formula of YV[a]P[1-a]O4:bCe<3+>, wherein YV[a]P[1-a]O4 is a matrix, Ce<3+> is an activation element, a is 0.1-0.6, and b is 0.01-0.05. In an electroluminescence (EL) spectrum of a luminescent thin film prepared from the cerium doped vanadium yttrium phosphate salt luminescent material, a wavelength region of 610 nm has very strong luminescence peaks, and the luminescent thin film can be used in a thin-film electroluminescent display. The invention also provides a preparation method and application of the cerium doped vanadium yttrium phosphate salt luminescent material.
Description
[technical field]
The present invention relates to a kind of cerium doping vanadium yttrium phosphate salt luminescent material, its preparation method, cerium doping vanadium yttrium phosphate salt light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof.
[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 is colored to be reached to panchromatic TFELD, and the luminous material of exploitation multiband, be the developing direction of this problem.But, can be applicable to the cerium doping vanadium yttrium phosphate salt luminescent material 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 cerium doping vanadium yttrium phosphate salt luminescent material, its preparation method, cerium doping vanadium yttrium phosphate salt light-emitting film, its preparation method that can be applicable to membrane electro luminescent device, use membrane electro luminescent device of this cerium doping vanadium yttrium phosphate salt luminescent material and preparation method thereof.
A kind of cerium doping vanadium yttrium phosphate salt luminescent material, its chemical formula is YV
aP
1-aO
4: bCe
3+, YV wherein
aP
1-aO
4Matrix, Ce
3+Ion is active element, and a is that 0.1～0.6, b is 0.01～0.05.
A kind of preparation method of cerium doping vanadium yttrium phosphate salt luminescent material comprises the following steps:
According to YV
aP
1-aO
4: bCe
3+The stoichiometric ratio of each element takes Y
2O
3, V
2O
5, P
2O
5, and CeO
2Powder also mixes, and wherein a is that 0.1～0.6, b is 0.01～0.05; And
The powder mixed is obtained to chemical formula in 0.5 hour～5 hours at 900 ℃～1300 ℃ lower sintering is YV
aP
1-aO
4: bCe
3+Cerium doping vanadium yttrium phosphate salt luminescent material.
A kind of cerium doping vanadium yttrium phosphate salt light-emitting film, the chemical general formula of the material of this cerium doping vanadium yttrium phosphate salt light-emitting film is YV
aP
1-aO
4: bCe
3+, YV wherein
aP
1-aO
4Matrix, Ce
3+Ion is active element, and a is that 0.1～0.6, b is 0.01～0.05.
A kind of preparation method of cerium doping vanadium yttrium phosphate salt light-emitting film comprises the following steps:
According to YV
aP
1-aO
4: bCe
3+The stoichiometric ratio of each element takes Y
2O
3, V
2O
5, P
2O
5, and CeO
2Powder also mixes at 900 ℃～1300 ℃ lower sintering and within 0.5 hour～5 hours, makes target, and wherein a is that 0.1～0.6, b is 0.01～0.05;
By pack into the vacuum cavity of magnetic-controlled sputtering coating equipment of described target and substrate, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3Pa～1.0 * 10
-5Pa; And
Adjusting the magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, and underlayer temperature is 250 ℃～750 ℃, then is filmed, and obtaining chemical formula is YV
aP
1-aO
4: bCe
3+Cerium doping vanadium yttrium phosphate salt light-emitting film.
In a preferred embodiment, also comprise step: described cerium doping vanadium yttrium phosphate salt light-emitting film is processed to 1h～3h in 500 ℃～800 ℃ lower vacuum annealings.
In a preferred embodiment, the vacuum tightness of described vacuum cavity is 5.0 * 10
-4Pa, base target spacing is 60mm, and the magnetron sputtering operating pressure is 2Pa, and working gas is argon gas, and the flow of working gas is 25sccm, underlayer temperature is 500 ℃.
A kind of membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer stacked gradually, the material of described luminescent layer is cerium doping vanadium yttrium phosphate salt luminescent material, and the chemical formula of this cerium doping vanadium yttrium phosphate salt luminescent material is YV
aP
1-aO
4: bCe
3+, YV wherein
aP
1-aO
4Matrix, Ce
3+Ion is active element, and a is that 0.1～0.6, b is 0.01～0.05.
A kind of preparation method of membrane electro luminescent device comprises the following steps:
Substrate with anode is provided;
Form luminescent layer on described anode, the material of described luminescent layer is cerium doping vanadium yttrium phosphate salt luminescent material, and the chemical formula of this cerium doping vanadium yttrium phosphate salt luminescent material is YV
aP
1-aO
4: bCe
3+, a is that 0.1～0.6, b is 0.01～0.05;
Form negative electrode on described luminescent layer.
In a preferred embodiment, the preparation of described luminescent layer comprises the following steps:
According to YV
aP
1-aO
4: bCe
3+The stoichiometric ratio of each element takes Y
2O
3, V
2O
5, P
2O
5, and CeO
2Powder also mixes at 900 ℃～1300 ℃ lower sintering and within 0.5 hour～5 hours, makes target, and wherein a is that 0.1～0.6, b is 0.01～0.05;
By pack into the vacuum cavity of magnetic-controlled sputtering coating equipment of described target and described substrate, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3Pa～1.0 * 10
-5Pa;
Adjusting the magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 ℃～750 ℃, then be filmed, on described anode, form luminescent layer.
In a preferred embodiment, the preparation of described luminescent layer also comprises step: described luminescent layer is processed to 1h～3h in 500 ℃～800 ℃ lower vacuum annealings.
Above-mentioned cerium doping vanadium yttrium phosphate salt luminescent material (YV
aP
1-aO
4: bCe
3+) in the electroluminescent spectrum (EL) of the light-emitting film made, at the 610nm wavelength zone, very strong glow peak being arranged, can be applied in thin-film electroluminescent displays.
[accompanying drawing explanation]
The structural representation of the membrane electro luminescent device that Fig. 1 is an embodiment;
The electroluminescent spectrogram of the cerium doping vanadium yttrium phosphate salt light-emitting film that Fig. 2 is embodiment 1 preparation;
The XRD figure of the cerium doping vanadium yttrium phosphate salt light-emitting film that Fig. 3 is embodiment 1 preparation;
Fig. 4 is the voltage of membrane electro luminescent device of embodiment 1 preparation and the graph of relation between current density and voltage and brightness.
[embodiment]
Below in conjunction with the drawings and specific embodiments, cerium doping vanadium yttrium phosphate salt luminescent material, its preparation method, cerium doping vanadium yttrium phosphate salt light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof are further illustrated.
The cerium doping vanadium yttrium phosphate salt luminescent material of one embodiment, its chemical formula is YV
aP
1-aO
4: bCe
3+, YV wherein
aP
1-aO
4Matrix, Ce
3+Ion is active element, and a is that 0.1～0.6, b is 0.01～0.05.
Preferably, a is that 0.3, b is 0.02.
YV in this cerium doping vanadium yttrium phosphate salt luminescent material
aP
1-aO
4Matrix, Ce
3+Ion is active element.In the electroluminescent spectrum (EL) of the light-emitting film that this cerium doping vanadium yttrium phosphate salt luminescent material is made, at the 610nm wavelength zone, very strong glow peak is arranged, can be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned cerium doping vanadium yttrium phosphate salt luminescent material comprises the following steps:
Step S11, according to YV
aP
1-aO
4: bCe
3+The stoichiometric ratio of each element takes Y
2O
3, V
2O
5, P
2O
5, and CeO
2Powder, wherein a is that 0.1～0.6, b is 0.01～0.05.
In this step, preferred, a is that 0.3, b is 0.02.
Step S12, will mix equal powder and within 0.5 hour～5 hours, can obtain cerium doping vanadium yttrium phosphate salt luminescent material at 900 ℃～1300 ℃ lower sintering, its chemical formula is YV
aP
1-aO
4: bCe
3+, YV wherein
aP
1-aO
4Matrix, Ce
3+Ion is active element, and a is that 0.1～0.6, b is 0.01～0.05.
In this step, preferably 1250 ℃ of lower sintering 3 hours.
The cerium doping vanadium yttrium phosphate salt light-emitting film of one embodiment, the chemical general formula of the material of this cerium doping vanadium yttrium phosphate salt light-emitting film is YV
aP
1-aO
4: bCe
3+, YV wherein
aP
1-aO
4Matrix, Ce
3+Ion is active element, and a is that 0.1～0.6, b is 0.01～0.05.
Preferably, a is that 0.3, b is 0.02.
The preparation method of above-mentioned cerium doping vanadium yttrium phosphate salt light-emitting film comprises the following steps:
Step S21, press YV
aP
1-aO
4: bCe
3+The stoichiometric ratio of each element takes Y
2O
3, V
2O
5, P
2O
5, and CeO
2Powder also mixes at 900 ℃～1300 ℃ lower sintering and within 0.5 hour～5 hours, makes target, and wherein a is that 0.1～0.6, b is 0.01～0.05.
In this step, preferred, a is that 0.3, b is 0.02, and within 3 hours, becoming diameter at 1250 ℃ of lower sintering is 50mm, the ceramic target that thickness is 2mm.
Step S22, by pack into the vacuum cavity of magnetic-controlled sputtering coating equipment of the target that obtains in 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: 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 ℃～750 ℃; Then be filmed, obtain cerium doping vanadium yttrium phosphate salt light-emitting film.
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 ℃.
Step S24, the cerium vanadium yttrium phosphate salt light-emitting film that adulterates is processed to 1h～3h in 500 ℃～800 ℃ lower vacuum annealings.
In this step, preferred, film sample is processed 2h 600 ℃ of lower vacuum annealings.
Refer to Fig. 1, the membrane electro luminescent device 100 of an embodiment, this membrane electro luminescent device 100 comprises substrate 1, anode 2, luminescent layer 3 and the negative electrode 4 stacked gradually.
Substrate 1 is glass substrate.Anode 2 is for being formed at the tin indium oxide (ITO) on glass substrate.The material of luminescent layer 3 is cerium doping vanadium yttrium phosphate salt luminescent material, and the chemical formula of this cerium doping vanadium yttrium phosphate salt luminescent material is YV
aP
1-aO
4: bCe
3+, a is that 0.1～0.6, b is 0.01～0.05.The material of negative electrode 4 is silver (Ag).
The preparation method of above-mentioned membrane electro luminescent device comprises the following steps:
Step S31, provide the substrate 1 with anode 2.
In present embodiment, substrate 1 is glass substrate, and anode 2 is for being formed at the tin indium oxide (ITO) on glass substrate.Substrate 1 with anode 2 is successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning and use it is carried out to oxygen plasma treatment.
Step S32, form luminescent layer 3 on anode 2, the material of luminescent layer 3 is cerium doping vanadium yttrium phosphate salt luminescent material, and the chemical formula of this cerium doping vanadium yttrium phosphate salt luminescent material is YV
aP
1-aO
4: bCe
3+, YV wherein
aP
1-aO
4Matrix, Ce
3+Ion is active element, and a is that 0.1～0.6, b is 0.01～0.05.
In present embodiment, luminescent layer 3 is made by following steps:
At first, by YV
aP
1-aO
4: bCe
3+The stoichiometric ratio of each element takes Y
2O
3, V
2O
5, P
2O
5, and CeO
2Powder also mixes at 900 ℃～1300 ℃ lower sintering and within 0.5 hour～5 hours, makes target, and wherein a is that 0.1～0.6, b is 0.01～0.05.
In this step, preferred, a is that 0.3, b is 0.02, and within 3 hours, becoming diameter at 1250 ℃ of lower sintering is 50mm, the ceramic target that thickness is 2mm.
Secondly, by pack into the vacuum cavity of magnetic-controlled sputtering coating equipment of target 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.
Then, adjusting the magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 ℃～750 ℃, then is filmed, and forms luminescent layer 3 on anode 2.
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 ℃.
Finally, luminescent layer 3 is processed to 1h～3h in 500 ℃～800 ℃ lower vacuum annealings.
In this step, preferred, film sample is processed 2h 600 ℃ of lower vacuum annealings.
Step S33, form negative electrode 4 on luminescent layer 3.
In present embodiment, the material of negative electrode 4 is silver (Ag), by evaporation, is formed.
It is below specific embodiment.
Embodiment 1
Select the powder that purity is 99.99%, by the Y of 0.5mol
2O
3, the V of 0.15mol
2O
5, the P of 0.35mol
2O
5CeO with 0.02mol
2, after even mixing, sintering diameter under 1250 ℃ into is 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 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 60mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into to 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 the obtained 2h that anneals in the 0.01Pa vacuum oven, annealing temperature is 600 ℃, obtaining chemical formula is YV
0.3P
0.7O
4: 0.02Ce
3+Light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
The chemical general formula of the cerium doping vanadium yttrium phosphate salt light-emitting film obtained in the present embodiment is YV
0.3P
0.7O
4: 0.02Ce
3+, YV wherein
0.3P
0.7O
4Matrix, Ce
3+Ion is active element.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the cerium doping vanadium yttrium phosphate salt light-emitting film obtained.As seen from Figure 2, in electroluminescence spectrum, at the 610nm wavelength zone, very strong glow peak is arranged, can be applied in thin-film electroluminescent displays.
Refer to Fig. 3, the XRD curve of the cerium doping vanadium yttrium phosphate salt light-emitting film that Fig. 3 is embodiment 1 preparation, test comparison standard P DF card.As can be seen from Figure 3, diffraction peak is all the peak crystallization that vanadium yttrium phosphate salt is relevant, the diffraction peak of doped element and other impurity do not occur.
Refer to Fig. 4, Fig. 4 is the voltage of membrane electro luminescent device of embodiment 1 preparation and the graph of relation between current density and voltage and brightness, curve 1 is voltage and current density relation curve, can find out that this device starts luminous from voltage 5.5V, curve 2 is voltage and brightness relationship curve, and the high-high brightness that can find out this device is 79cd/m
2, show that device has the good characteristics of luminescence.
Embodiment 2
Select the powder that purity is 99.99%, by the Y of 0.5mol
2O
3, the V of 0.05mol
2O
5, the P of 0.45mol
2O
5CeO with 0.01mol
2, after even mixing, sintering diameter under 900 ℃ into is 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 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.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into to 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 the obtained 1h that anneals in the 0.01Pa vacuum oven, annealing temperature is 500 ℃.Obtaining chemical formula is YV
0.1P
0.9O
4: 0.01Ce
3+Light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 3
Select the powder that purity is 99.99%, by the Y of 0.5mol
2O
3, the V of 0.3mol
2O
5, the P of 0.2mol
2O
5CeO with 0.05mol
2, after even mixing, sintering diameter under 1300 ℃ into is 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 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.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into to 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 the obtained 3h that anneals in the 0.01Pa vacuum oven, annealing temperature is 800 ℃.Obtaining chemical formula is YV
0.6P
0.4O
4: 0.05Ce
3+Light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Select the powder that purity is 99.99%, by the Y of 0.5mol
2O
3, the V of 0.1mol
2O
5, the P of 0.4mol
2O
5CeO with 0.03mol
2, after even mixing, sintering diameter under 1250 ℃ into is 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 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 60mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into to 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 the obtained 2h that anneals in the 0.01Pa vacuum oven, annealing temperature is 600 ℃.Obtaining chemical formula is YV
0.2P
0.8O
4: 0.03Ce
3+Light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 5
Select the powder that purity is 99.99%, by the Y of 0.5mol
2O
3, the V of 0.2mol
2O
5, the P of 0.3mol
2O
5CeO with 0.04mol
2, after even mixing, sintering diameter under 900 ℃ into is 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 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.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into to 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 the obtained 1h that anneals in the 0.01Pa vacuum oven, annealing temperature is 500 ℃.Obtaining chemical formula is YV
0.4P
0.6O
4: 0.04Ce
3+Light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Select the powder that purity is 99.99%, by the Y of 0.5mol
2O
3, the V of 0.25mol
2O
5, the P of 0.25mol
2O
5CeO with 0.04mol
2, after even mixing, sintering diameter under 1300 ℃ into is 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 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.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into to 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 the obtained 3h that anneals in the 0.01Pa vacuum oven, annealing temperature is 800 ℃.Obtaining chemical formula is YV
0.5P
0.5O
4: 0.04Ce
3+Light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 7
Select the powder that purity is 99.99%, by the Y of 0.5mol
2O
3, the V of 0.125mol
2O
5, the P of 0.375mol
2O
5CeO with 0.02mol
2, after even mixing, sintering diameter under 1250 ℃ into is 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 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 60mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into to 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 the obtained 2h that anneals in the 0.01Pa vacuum oven, annealing temperature is 600 ℃.Obtaining chemical general formula is YV
0.25P
0.75O
4: 0.02Ce
3+Light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. cerium doping vanadium yttrium phosphate salt luminescent material, it is characterized in that: its chemical formula is YV
aP
1-aO
4: bCe
3+, YV wherein
aP
1-aO
4Matrix, Ce
3+Ion is active element, and a is that 0.1～0.6, b is 0.01～0.05.
2. the preparation method of a cerium doping vanadium yttrium phosphate salt luminescent material, is characterized in that, comprises the following steps:
According to YV
aP
1-aO
4: bCe
3+The stoichiometric ratio of each element takes Y
2O
3, V
2O
5, P
2O
5, and CeO
2Powder also mixes, and wherein a is that 0.1～0.6, b is 0.01～0.05; And
The powder mixed is obtained to chemical formula in 0.5 hour～5 hours at 900 ℃～1300 ℃ lower sintering is YV
aP
1-aO
4: bCe
3+Cerium doping vanadium yttrium phosphate salt luminescent material.
3. a cerium doping vanadium yttrium phosphate salt light-emitting film, is characterized in that, the chemical general formula of the material of this cerium doping vanadium yttrium phosphate salt light-emitting film is YV
aP
1-aO
4: bCe
3+, YV wherein
aP
1-aO
4Matrix, Ce
3+Ion is active element, and a is that 0.1～0.6, b is 0.01～0.05.
4. the preparation method of a cerium doping vanadium yttrium phosphate salt light-emitting film, is characterized in that, comprises the following steps:
According to YV
aP
1-aO
4: bCe
3+The stoichiometric ratio of each element takes Y
2O
3, V
2O
5, P
2O
5, and CeO
2Powder also mixes at 900 ℃～1300 ℃ lower sintering and makes target in 0.5 hour～5 hours, and wherein, a is that 0.1～0.6, b is 0.01～0.05;
By pack into the vacuum cavity of magnetic-controlled sputtering coating equipment of described target and substrate, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3Pa～1.0 * 10
-5Pa; And
Adjusting the magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, and underlayer temperature is 250 ℃～750 ℃, then is filmed, and obtaining chemical formula is YV
aP
1-aO
4: bCe
3+Cerium doping vanadium yttrium phosphate salt light-emitting film.
5. the preparation method of cerium doping vanadium yttrium phosphate salt light-emitting film according to claim 4, is characterized in that, also comprises step: described cerium doping vanadium yttrium phosphate salt light-emitting film is processed to 1h～3h in 500 ℃～800 ℃ lower vacuum annealings.
6. the preparation method of cerium doping vanadium yttrium phosphate salt light-emitting film according to claim 4, is characterized in that, the vacuum tightness of described vacuum cavity is 5.0 * 10
-4Pa, base target spacing is 60mm, and the magnetron sputtering operating pressure is 2Pa, and working gas is argon gas, and the flow of working gas is 25sccm, underlayer temperature is 500 ℃.
7. a membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer stacked gradually, it is characterized in that, the material of described luminescent layer is cerium doping vanadium yttrium phosphate salt luminescent material, and the chemical formula of this cerium doping vanadium yttrium phosphate salt luminescent material is YV
aP
1-aO
4: bCe
3+, YV wherein
aP
1-aO
4Matrix, Ce
3+Ion is active element, and a is that 0.1～0.6, b is 0.01～0.05.
8. the preparation method of a membrane electro luminescent device, is characterized in that, comprises the following steps:
Substrate with anode is provided;
Form luminescent layer on described anode, the material of described luminescent layer is cerium doping vanadium yttrium phosphate salt luminescent material, and the chemical formula of this cerium doping vanadium yttrium phosphate salt luminescent material is YV
aP
1-aO
4: bCe
3+, a is that 0.1～0.6, b is 0.01～0.05;
Form negative electrode on described luminescent layer.
9. the preparation method of membrane electro luminescent device according to claim 8, is characterized in that, the preparation of described luminescent layer comprises the following steps:
According to YV
aP
1-aO
4: bCe
3+The stoichiometric ratio of each element takes Y
2O
3, V
2O
5, P
2O
5, and CeO
2Powder also mixes at 900 ℃～1300 ℃ lower sintering and within 0.5 hour～5 hours, makes target, and wherein a is that 0.1～0.6, b is 0.01～0.05;
By pack into the vacuum cavity of magnetic-controlled sputtering coating equipment of described target and described substrate, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3Pa～1.0 * 10
-5Pa;
Adjusting the magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 ℃～750 ℃, then be filmed, on described anode, form luminescent layer.
10. the preparation method of membrane electro luminescent device according to claim 9, is characterized in that, the preparation of described luminescent layer also comprises step: described luminescent layer is processed to 1h～3h in 500 ℃～800 ℃ lower vacuum annealings.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010108815A1 (en) * | 2009-03-24 | 2010-09-30 | Rhodia Operations | Core/shell lanthanum cerium terbium phosphate, phosphor containing said phosphate, and preparation methods |
| CN101974334A (en) * | 2010-09-25 | 2011-02-16 | 西安理工大学 | Single-phase rare earth vanadium phosphate white fluorescent powder for mercury lamp and preparation method thereof |
| CN102443394A (en) * | 2010-10-11 | 2012-05-09 | 海洋王照明科技股份有限公司 | Vanadium phosphate phosphor and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010108815A1 (en) * | 2009-03-24 | 2010-09-30 | Rhodia Operations | Core/shell lanthanum cerium terbium phosphate, phosphor containing said phosphate, and preparation methods |
| CN101974334A (en) * | 2010-09-25 | 2011-02-16 | 西安理工大学 | Single-phase rare earth vanadium phosphate white fluorescent powder for mercury lamp and preparation method thereof |
| CN102443394A (en) * | 2010-10-11 | 2012-05-09 | 海洋王照明科技股份有限公司 | Vanadium phosphate phosphor and preparation method thereof |
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