CN103421509B - Cerium dopping vanadium yttrium phosphate salt luminescent material, preparation method and application thereof - Google Patents
Cerium dopping vanadium yttrium phosphate salt luminescent material, preparation method and application thereof Download PDFInfo
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Abstract
A kind of cerium dopping vanadium yttrium phosphate salt luminescent material, its chemical formula is YV
ap
1-ao
4: bCe
3+, wherein YV
ap
1-ao
4matrix, Ce
3+ion is active element, and a is 0.1 ~ 0.6, b is 0.01 ~ 0.05.In the electroluminescent spectrum (EL) of the light-emitting film that this cerium dopping vanadium yttrium phosphate salt luminescent material is made, there is very strong glow peak in 610nm wavelength zone, can be applied in thin-film electroluminescent displays.The present invention also provides preparation method and the application thereof of this cerium dopping vanadium yttrium phosphate salt luminescent material.
Description
[technical field]
The present invention relates to a kind of cerium dopping vanadium yttrium phosphate salt luminescent material, its preparation method, cerium dopping 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 colour and extremely panchromatic TFELD, the material of exploitation multiband luminescence is the developing direction of this problem.But, can be applicable to the cerium dopping 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 the cerium dopping vanadium yttrium phosphate salt luminescent material, its preparation method, cerium dopping vanadium yttrium phosphate salt light-emitting film, its preparation method, the membrane electro luminescent device using this cerium dopping vanadium yttrium phosphate salt luminescent material and preparation method thereof that can be applicable to membrane electro luminescent device.
A kind of cerium dopping vanadium yttrium phosphate salt luminescent material, its chemical formula is YV
ap
1-ao
4: bCe
3+, wherein YV
ap
1-ao
4matrix, Ce
3+ion is active element, and a is 0.1 ~ 0.6, b is 0.01 ~ 0.05.
A preparation method for cerium dopping 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 0.1 ~ 0.6, b is 0.01 ~ 0.05; And
Namely the powder mixed sinter 0.5 hour ~ 5 hours to be obtained chemical formula being YV at 900 DEG C ~ 1300 DEG C
ap
1-ao
4: bCe
3+cerium dopping vanadium yttrium phosphate salt luminescent material.
A kind of cerium dopping vanadium yttrium phosphate salt light-emitting film, the chemical general formula of the material of this cerium dopping vanadium yttrium phosphate salt light-emitting film is YV
ap
1-ao
4: bCe
3+, wherein YV
ap
1-ao
4matrix, Ce
3+ion is active element, and a is 0.1 ~ 0.6, b is 0.01 ~ 0.05.
A preparation method for cerium dopping 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 to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, and wherein a is 0.1 ~ 0.6, b is 0.01 ~ 0.05;
Described target and substrate are loaded 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; And
Adjustment 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 DEG C ~ 750 DEG C, is then filmed, and obtaining chemical formula is YV
ap
1-ao
4: bCe
3+cerium dopping vanadium yttrium phosphate salt light-emitting film.
In a preferred embodiment, also step is comprised: by described cerium dopping vanadium yttrium phosphate salt light-emitting film vacuum annealing process 1h ~ 3h at 500 DEG C ~ 800 DEG C.
In a preferred embodiment, the vacuum tightness of described vacuum cavity is 5.0 × 10
-4pa, base target spacing is 60mm, and magnetron sputtering operating pressure is 2Pa, and working gas is argon gas, and the flow of working gas is 25sccm, and underlayer temperature is 500 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 cerium dopping vanadium yttrium phosphate salt luminescent material, and the chemical formula of this cerium dopping vanadium yttrium phosphate salt luminescent material is YV
ap
1-ao
4: bCe
3+, wherein YV
ap
1-ao
4matrix, Ce
3+ion is active element, and a is 0.1 ~ 0.6, b is 0.01 ~ 0.05.
A preparation method for membrane electro luminescent device, comprises the following steps:
The substrate with anode is provided;
Described anode forms luminescent layer, and the material of described luminescent layer is cerium dopping vanadium yttrium phosphate salt luminescent material, and the chemical formula of this cerium dopping vanadium yttrium phosphate salt luminescent material is YV
ap
1-ao
4: bCe
3+, a is 0.1 ~ 0.6, b is 0.01 ~ 0.05;
Form negative electrode on the light-emitting 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 to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, and wherein a is 0.1 ~ 0.6, b is 0.01 ~ 0.05;
Described target and described substrate are loaded 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;
Adjustment 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, and underlayer temperature is 250 DEG C ~ 750 DEG C, then be filmed, described anode forms luminescent layer.
In a preferred embodiment, the preparation of described luminescent layer also comprises step: by described luminescent layer vacuum annealing process 1h ~ 3h at 500 DEG C ~ 800 DEG C.
Above-mentioned cerium dopping vanadium yttrium phosphate salt luminescent material (YV
ap
1-ao
4: bCe
3+) in the electroluminescent spectrum (EL) of light-emitting film made, have very strong glow peak in 610nm wavelength zone, can be applied in thin-film electroluminescent displays.
[accompanying drawing explanation]
Fig. 1 is the structural representation of the membrane electro luminescent device of an embodiment;
Fig. 2 is the electroluminescent spectrogram of cerium dopping vanadium yttrium phosphate salt light-emitting film prepared by embodiment 1;
Fig. 3 is the XRD figure of cerium dopping vanadium yttrium phosphate salt light-emitting film prepared by embodiment 1;
Fig. 4 is the voltage of membrane electro luminescent device prepared of embodiment 1 and current density and the graph of relation between voltage and brightness.
[embodiment]
Below in conjunction with the drawings and specific embodiments, cerium dopping vanadium yttrium phosphate salt luminescent material, its preparation method, cerium dopping vanadium yttrium phosphate salt light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof are illustrated further.
The cerium dopping vanadium yttrium phosphate salt luminescent material of one embodiment, its chemical formula is YV
ap
1-ao
4: bCe
3+, wherein YV
ap
1-ao
4matrix, Ce
3+ion is active element, and a is 0.1 ~ 0.6, b is 0.01 ~ 0.05.
Preferably, a is 0.3, b is 0.02.
YV in this cerium dopping 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 dopping vanadium yttrium phosphate salt luminescent material is made, there is very strong glow peak in 610nm wavelength zone, can be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned cerium dopping 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 0.1 ~ 0.6, b is 0.01 ~ 0.05.
In this step, preferably, a is 0.3, b is 0.02.
Step S12, the equal powder of mixing is sintered 0.5 hour ~ 5 hours and can obtain cerium dopping vanadium yttrium phosphate salt luminescent material at 900 DEG C ~ 1300 DEG C, its chemical formula is YV
ap
1-ao
4: bCe
3+, wherein YV
ap
1-ao
4matrix, Ce
3+ion is active element, and a is 0.1 ~ 0.6, b is 0.01 ~ 0.05.
In this step, preferably at 1250 DEG C, sinter 3 hours.
The cerium dopping vanadium yttrium phosphate salt light-emitting film of one embodiment, the chemical general formula of the material of this cerium dopping vanadium yttrium phosphate salt light-emitting film is YV
ap
1-ao
4: bCe
3+, wherein YV
ap
1-ao
4matrix, Ce
3+ion is active element, and a is 0.1 ~ 0.6, b is 0.01 ~ 0.05.
Preferably, a is 0.3, b is 0.02.
The preparation method of above-mentioned cerium dopping vanadium yttrium phosphate salt light-emitting film, comprises the following steps:
Step S21, 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 to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, and wherein a is 0.1 ~ 0.6, b is 0.01 ~ 0.05.
In this step, preferably, a is 0.3, b is 0.02, and at 1250 DEG C, sinter 3 hours become diameter to be 50mm, thickness is the ceramic target of 2mm.
Step S22, the target that obtains in step S21 and substrate are loaded 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, preferably, 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, and underlayer temperature is 250 DEG C ~ 750 DEG C; Then be filmed, obtain cerium dopping 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 DEG C.
Step S24, by cerium dopping vanadium yttrium phosphate salt light-emitting film vacuum annealing process 1h ~ 3h at 500 DEG C ~ 800 DEG C.
In this step, preferably, film sample vacuum annealing process 2h at 600 DEG C.
Refer to Fig. 1, the membrane electro luminescent device 100 of an embodiment, this membrane electro luminescent device 100 comprises the substrate 1, anode 2, luminescent layer 3 and the negative electrode 4 that stack gradually.
Substrate 1 is glass substrate.Anode 2 is for being formed at the tin indium oxide (ITO) in glass substrate.The material of luminescent layer 3 is cerium dopping vanadium yttrium phosphate salt luminescent material, and the chemical formula of this cerium dopping vanadium yttrium phosphate salt luminescent material is YV
ap
1-ao
4: bCe
3+, a is 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) in glass substrate.There is the substrate 1 priority acetone of anode 2, dehydrated alcohol and deionized water ultrasonic cleaning and carry out oxygen plasma treatment with to it.
Step S32, on anode 2, form luminescent layer 3, the material of luminescent layer 3 is cerium dopping vanadium yttrium phosphate salt luminescent material, and the chemical formula of this cerium dopping vanadium yttrium phosphate salt luminescent material is YV
ap
1-ao
4: bCe
3+, wherein YV
ap
1-ao
4matrix, Ce
3+ion is active element, and a is 0.1 ~ 0.6, b is 0.01 ~ 0.05.
In present embodiment, luminescent layer 3 is obtained by following steps:
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 to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, and wherein a is 0.1 ~ 0.6, b is 0.01 ~ 0.05.
In this step, preferably, a is 0.3, b is 0.02, and at 1250 DEG C, sinter 3 hours become diameter to be 50mm, thickness is the ceramic target of 2mm.
Secondly, target and substrate are loaded 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, preferably, vacuum tightness is 5 × 10
-4pa.
Then, adjusting 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 DEG C ~ 750 DEG C, is then filmed, and anode 2 is formed luminescent layer 3.
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.
Finally, by luminescent layer 3 vacuum annealing process 1h ~ 3h at 500 DEG C ~ 800 DEG C.
In this step, preferably, film sample vacuum annealing process 2h at 600 DEG C.
Step S33, on luminescent layer 3, form negative electrode 4.
In present embodiment, the material of negative electrode 4 is silver (Ag), is formed by evaporation.
Be specific embodiment below.
Embodiment 1
Select purity be 99.99% powder, by the Y of 0.5mol
2o
3, the V of 0.15mol
2o
5, the P of 0.35mol
2o
5with the CeO of 0.02mol
2, after Homogeneous phase mixing, at 1250 DEG C, sinter diameter into is 50mm, and thickness is the ceramic target of 2mm, and is loaded in vacuum cavity by target.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and carry out oxygen plasma treatment with to it, 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 DEG C.The sample obtained is annealed 2h in 0.01Pa vacuum oven, and annealing temperature is 600 DEG C, and obtaining chemical formula is YV
0.3p
0.7o
4: 0.02Ce
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula of the cerium dopping vanadium yttrium phosphate salt light-emitting film obtained in the present embodiment is YV
0.3p
0.7o
4: 0.02Ce
3+, wherein YV
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 dopping vanadium yttrium phosphate salt light-emitting film obtained.As seen from Figure 2, in electroluminescence spectrum, there is very strong glow peak in 610nm wavelength zone, can be applied in thin-film electroluminescent displays.
Refer to Fig. 3, Fig. 3 is the XRD curve of cerium dopping vanadium yttrium phosphate salt light-emitting film prepared by embodiment 1, 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, does not occur the diffraction peak of doped element and other impurity.
Refer to Fig. 4, Fig. 4 is the voltage of membrane electro luminescent device prepared of embodiment 1 and current density and the graph of relation between voltage and brightness, curve 1 is voltage and current density relation curve, the luminescence from voltage 5.5V of this device can be found out, curve 2 is voltage and brightness relationship curve, can find out that the high-high brightness of this device is 79cd/m
2, show that device has the good characteristics of luminescence.
Embodiment 2
Select purity be 99.99% powder, by the Y of 0.5mol
2o
3, the V of 0.05mol
2o
5, the P of 0.45mol
2o
5with the CeO of 0.01mol
2, after Homogeneous phase mixing, at 900 DEG C, sinter diameter into is 50mm, and thickness is the ceramic target of 2mm, and is loaded in vacuum cavity by target.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and carry out oxygen plasma treatment with to it, 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 DEG C.The sample obtained is annealed 1h in 0.01Pa vacuum oven, and annealing temperature is 500 DEG C.Obtaining chemical formula is YV
0.1p
0.9o
4: 0.01Ce
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 3
Select purity be 99.99% powder, by the Y of 0.5mol
2o
3, the V of 0.3mol
2o
5, the P of 0.2mol
2o
5with the CeO of 0.05mol
2, after Homogeneous phase mixing, at 1300 DEG C, sinter diameter into is 50mm, and thickness is the ceramic target of 2mm, and is loaded in vacuum cavity by target.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and carry out oxygen plasma treatment with to it, 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 DEG C.The sample obtained is annealed 3h in 0.01Pa vacuum oven, and annealing temperature is 800 DEG C.Obtaining chemical formula is YV
0.6p
0.4o
4: 0.05Ce
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 4
Select purity be 99.99% powder, by the Y of 0.5mol
2o
3, the V of 0.1mol
2o
5, the P of 0.4mol
2o
5with the CeO of 0.03mol
2, after Homogeneous phase mixing, at 1250 DEG C, sinter diameter into is 50mm, and thickness is the ceramic target of 2mm, and is loaded in vacuum cavity by target.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and carry out oxygen plasma treatment with to it, 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 DEG C.The sample obtained is annealed 2h in 0.01Pa vacuum oven, and annealing temperature is 600 DEG C.Obtaining chemical formula is YV
0.2p
0.8o
4: 0.03Ce
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 5
Select purity be 99.99% powder, by the Y of 0.5mol
2o
3, the V of 0.2mol
2o
5, the P of 0.3mol
2o
5with the CeO of 0.04mol
2, after Homogeneous phase mixing, at 900 DEG C, sinter diameter into is 50mm, and thickness is the ceramic target of 2mm, and is loaded in vacuum cavity by target.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and carry out oxygen plasma treatment with to it, 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 DEG C.The sample obtained is annealed 1h in 0.01Pa vacuum oven, and annealing temperature is 500 DEG C.Obtaining chemical formula is YV
0.4p
0.6o
4: 0.04Ce
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 6
Select purity be 99.99% powder, by the Y of 0.5mol
2o
3, the V of 0.25mol
2o
5, the P of 0.25mol
2o
5with the CeO of 0.04mol
2, after Homogeneous phase mixing, at 1300 DEG C, sinter diameter into is 50mm, and thickness is the ceramic target of 2mm, and is loaded in vacuum cavity by target.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and carry out oxygen plasma treatment with to it, 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 DEG C.The sample obtained is annealed 3h in 0.01Pa vacuum oven, and annealing temperature is 800 DEG C.Obtaining chemical formula is YV
0.5p
0.5o
4: 0.04Ce
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 7
Select purity be 99.99% powder, by the Y of 0.5mol
2o
3, the V of 0.125mol
2o
5, the P of 0.375mol
2o
5with the CeO of 0.02mol
2, after Homogeneous phase mixing, at 1250 DEG C, sinter diameter into is 50mm, and thickness is the ceramic target of 2mm, and is loaded in vacuum cavity by target.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and carry out oxygen plasma treatment with to it, 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 DEG C.The sample obtained is annealed 2h in 0.01Pa vacuum oven, and annealing temperature is 600 DEG C.Obtaining chemical general formula is YV
0.25p
0.75o
4: 0.02Ce
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not 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 (9)
1. a cerium dopping vanadium yttrium phosphate salt luminescent material, is characterized in that: its chemical formula is YV
ap
1-ao
4: bCe
3+, wherein YV
ap
1-ao
4matrix, Ce
3+ion is active element, and a is 0.1 ~ 0.6, b is 0.01 ~ 0.05.
2. a preparation method for cerium dopping 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 0.1 ~ 0.6, b is 0.01 ~ 0.05; And
Namely the powder mixed sinter 0.5 hour ~ 5 hours to be obtained chemical formula being YV at 900 DEG C ~ 1300 DEG C
ap
1-ao
4: bCe
3+cerium dopping vanadium yttrium phosphate salt luminescent material.
3. a cerium dopping vanadium yttrium phosphate salt light-emitting film, is characterized in that, the chemical general formula of the material of this cerium dopping vanadium yttrium phosphate salt light-emitting film is YV
ap
1-ao
4: bCe
3+, wherein YV
ap
1-ao
4matrix, Ce
3+ion is active element, and a is 0.1 ~ 0.6, b is 0.01 ~ 0.05.
4. a preparation method for cerium dopping 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 to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, and wherein, a is 0.1 ~ 0.6, b is 0.01 ~ 0.05;
Described target and substrate are loaded 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; And
Adjustment 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 DEG C ~ 750 DEG C, is then filmed, and obtaining chemical formula is YV
ap
1-ao
4: bCe
3+cerium dopping vanadium yttrium phosphate salt light-emitting film.
5. the preparation method of cerium dopping vanadium yttrium phosphate salt light-emitting film according to claim 4, is characterized in that, also comprise step: by described cerium dopping vanadium yttrium phosphate salt light-emitting film vacuum annealing process 1h ~ 3h at 500 DEG C ~ 800 DEG C.
6. the preparation method of cerium dopping 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 magnetron sputtering operating pressure is 2Pa, and working gas is argon gas, and the flow of working gas is 25sccm, and underlayer temperature is 500 DEG C.
7. 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 cerium dopping vanadium yttrium phosphate salt luminescent material, and the chemical formula of this cerium dopping vanadium yttrium phosphate salt luminescent material is YV
ap
1-ao
4: bCe
3+, wherein YV
ap
1-ao
4matrix, Ce
3+ion is active element, and a is 0.1 ~ 0.6, b is 0.01 ~ 0.05.
8. a preparation method for membrane electro luminescent device, is characterized in that, comprises the following steps:
The substrate with anode is provided;
Described anode forms luminescent layer, and the material of described luminescent layer is cerium dopping vanadium yttrium phosphate salt luminescent material, and the chemical formula of this cerium dopping vanadium yttrium phosphate salt luminescent material is YV
ap
1-ao
4: bCe
3+, a is 0.1 ~ 0.6, b is 0.01 ~ 0.05;
Form negative electrode on the light-emitting layer;
Wherein, 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 to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, and wherein a is 0.1 ~ 0.6, b is 0.01 ~ 0.05;
Described target and described substrate are loaded 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;
Adjustment 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, and underlayer temperature is 250 DEG C ~ 750 DEG C, then be filmed, described anode forms 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 also comprises step: by described luminescent layer vacuum annealing process 1h ~ 3h at 500 DEG C ~ 800 DEG C.
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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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