CN104650869A - Europium- terbium- co-doped aluminium niobate luminescent materials, and preparing method and applications thereof - Google Patents
Europium- terbium- co-doped aluminium niobate luminescent materials, and preparing method and applications thereof Download PDFInfo
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Abstract
Europium- terbium- co-doped aluminium niobate luminescent materials are provided. The general chemical formula of the materials is MeAl<1-x-y>NbO5:xEu<3+>,yTb<3+>, wherein the MeAl<1-x-y>NbO5 is a matrix, the Eu<3+> and the Bi<3+> are activating elements, the x is 0.01-0.08, the y is 0.01-0.06, and the Me is one of calcium, strontium and barium. In an electroluminescence spectrum (EL) of luminescent film prepared from one of the materials, strong luminescence peaks are obtained at 490 nm and 510 nm. The materials can be used in thin film electroluminescence displays. A preparing method and applications of the europium- terbium- co-doped aluminium niobate luminescent materials are also provided.
Description
[technical field]
The present invention relates to a kind of europium terbium codoped aluminium niobate luminescent material, its preparation method, europium terbium codoped aluminium niobate 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 europium terbium codoped aluminium niobate 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 europium terbium codoped aluminium niobate luminescent material, its preparation method, europium terbium codoped aluminium niobate light-emitting film, its preparation method, the membrane electro luminescent device using this europium terbium codoped aluminium niobate luminescent material and preparation method thereof that can be applicable to membrane electro luminescent device.
A kind of europium terbium codoped aluminium niobate luminescent material, its chemical formula is MeAl
1-x-ynbO
5: xEu
3+, yTb
3+, MeAl
1-x-ynbO
5matrix, Eu
3+and Tb
3+ion is active element, wherein, and to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y.
Described x is 0.04, y is 0.03.
A preparation method for europium terbium codoped aluminium niobate luminescent material, comprises the following steps:
According to MeAl
1-x-ynbO
5: xEu
3+, yTb
3+the stoichiometric ratio of each element takes MeO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder also mixes, wherein, and to be 0.01 ~ 0.06, MeO be in calcium oxide, strontium oxide and barium oxide one that x is 0.01 ~ 0.08, y; And
Namely the powder mixed sinter 0.5 hour ~ 5 hours to be obtained chemical formula being MeAl at 900 DEG C ~ 1300 DEG C
1-x-ynbO
5: xEu
3+, yTb
3+europium terbium codoped aluminium niobate luminescent material, to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y.
A kind of europium terbium codoped aluminium niobate light-emitting film, the chemical general formula of the material of this europium terbium codoped aluminium niobate light-emitting film is MeAl
1-x-ynbO
5: xEu
3+, yTb
3+, MeAl
1-x-ynbO
5matrix, Eu
3+and Tb
3+ion is active element, wherein, and to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y.
A preparation method for europium terbium codoped aluminium niobate light-emitting film, comprises the following steps:
According to MeAl
1-x-ynbO
5: xEu
3+, yTb
3+the stoichiometric ratio of each element takes MeO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder also mixes, and the powder mixed is sintered 0.5 hour ~ 5 hours at 900 DEG C ~ 1300 DEG C and obtains target, wherein, and to be 0.01 ~ 0.06, MeO be in calcium oxide, strontium oxide and barium oxide one that x is 0.01 ~ 0.08, y;
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 MeAl
1-x-ynbO
5: xEu
3+, yTb
3+europium terbium codoped aluminium niobate light-emitting film, to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y.
The preparation method of described europium terbium codoped aluminium niobate light-emitting film, also comprises step: by described europium terbium codoped aluminium niobate light-emitting film vacuum annealing process 1h ~ 3h at 500 DEG C ~ 800 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, it is characterized in that, the material of described luminescent layer is europium terbium codoped aluminium niobate luminescent material, and the chemical formula of this europium terbium codoped aluminium niobate luminescent material is MeAl
1-x-ynbO
5: xEu
3+, yTb
3+, MeAl
1-x-ynbO
5matrix, Eu
3+and Tb
3+ion is active element, wherein, and to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y.
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 europium terbium codoped aluminium niobate luminescent material, and the chemical formula of this europium terbium codoped aluminium niobate luminescent material is MeAl
1-x-ynbO
5: xEu
3+, yTb
3+, MeAl
1-x-ynbO
5matrix, Eu
3+and Tb
3+ion is active element, wherein, and to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y;
Form negative electrode on the light-emitting layer.
The preparation method of described membrane electro luminescent device, the preparation of described luminescent layer comprises the following steps:
According to MeAl
1-x-ynbO
5: xEu
3+, yTb
3+the stoichiometric ratio of each element takes MeO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder also to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, wherein, and to be 0.01 ~ 0.06, MeO be in calcium oxide, strontium oxide and barium oxide one that x is 0.01 ~ 0.08, y;
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.
The preparation method of described membrane electro luminescent device, also comprises step: by described europium terbium codoped aluminium niobate light-emitting film vacuum annealing process 1h ~ 3h at 500 DEG C ~ 800 DEG C.
Above-mentioned europium terbium codoped aluminium niobate luminescent material (MeAl
1-x-ynbO
5: xEu
3+, yTb
3+) in the electroluminescent spectrum (EL) of light-emitting film made, have very strong glow peak in 490nm and 510nm 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 europium terbium codoped aluminium niobate light-emitting film prepared by embodiment 1;
Fig. 3 is the XRD figure of europium terbium codoped aluminium niobate 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, europium terbium codoped aluminium niobate luminescent material, its preparation method, europium terbium codoped aluminium niobate light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof are illustrated further.
The europium terbium codoped aluminium niobate luminescent material of one embodiment, its chemical formula is MeAl
1-x-ynbO
5: xEu
3+, yTb
3+, MeAl
1-x-ynbO
5matrix, Eu
3+and Tb
3+ion is active element, wherein, and to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y.
Preferably, x is 0.04, y is 0.03.
In the electroluminescent spectrum (EL) of the light-emitting film that this europium terbium codoped aluminium niobate luminescent material is made, there is very strong glow peak in 490nm and 510nm wavelength zone, can be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned europium terbium codoped aluminium niobate luminescent material, comprises the following steps:
Step S11, according to MeAl
1-x-ynbO
5: xEu
3+, yTb
3+the stoichiometric ratio of each element takes MeO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder also mixes, wherein, and to be 0.01 ~ 0.06, MeO be in calcium oxide, strontium oxide and barium oxide one that x is 0.01 ~ 0.08, y; And
Namely the powder mixed sinter 0.5 hour ~ 5 hours to be obtained chemical formula being MeAl at 900 DEG C ~ 1300 DEG C
1-x-ynbO
5: xEu
3+, yTb
3+europium terbium codoped aluminium niobate luminescent material.
In this step, preferably, x is 0.04, y is 0.03.
Step S12, the equal powder of mixing is sintered 0.5 hour ~ 5 hours and can obtain europium terbium codoped aluminium niobate luminescent material at 900 DEG C ~ 1300 DEG C, its chemical formula is MeAl
1-x-ynbO
5: xEu
3+, yTb
3+.
In this step, preferably at 1250 DEG C, sinter 3 hours.
The europium terbium codoped aluminium niobate light-emitting film of one embodiment, the chemical general formula of the material of this europium terbium codoped aluminium niobate light-emitting film is MeAl
1-x-ynbO
5: xEu
3+, yTb
3+, MeAl
1-x-ynbO
5matrix, Eu
3+and Tb
3+ion is active element, wherein, and to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y.
Preferably, x is 0.04, y is 0.03.
The preparation method of above-mentioned europium terbium codoped aluminium niobate light-emitting film, comprises the following steps:
Step S21, by MeAl
1-x-ynbO
5: xEu
3+, yTb
3+the stoichiometric ratio of each element takes MeO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder also mixes, wherein, and to be 0.01 ~ 0.06, MeO be in calcium oxide, strontium oxide and barium oxide one that x is 0.01 ~ 0.08, y.
In this step, preferably, x is 0.04, y is 0.03, 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, obtaining chemical formula is MeAl
1-x-ynbO
5: xEu
3+, yTb
3+europium terbium codoped aluminium niobate light-emitting film.
Also comprise step: by described europium terbium codoped aluminium niobate light-emitting film vacuum annealing process 1h ~ 3h at 500 DEG C ~ 800 DEG C.
In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 2Pa, and working gas is oxygen, and the flow of working gas is 25sccm, and underlayer temperature is 500 DEG C.
Refer to Fig. 1, the membrane electro luminescent device of an embodiment, this membrane electro luminescent device 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 europium terbium codoped aluminium niobate luminescent material, and the chemical formula of this europium terbium codoped aluminium niobate luminescent material is MeAl
1-x-ynbO
5: xEu
3+, yTb
3+, MeAl
1-x-ynbO
5matrix, Eu
3+and Tb
3+ion is active element, wherein, and to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y.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 europium terbium codoped aluminium niobate luminescent material, and the chemical formula of this europium terbium codoped aluminium niobate luminescent material is MeAl
1-x-ynbO
5: xEu
3+, yTb
3+, MeAl
1-x-ynbO
5matrix, Eu
3+and Tb
3+ion is active element, and wherein, x is 0.01 ~ 0.08,
ythe one that to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element.
In present embodiment, luminescent layer 3 is obtained by following steps:
First, by MeAl
1-x-ynbO
5: xEu
3+, yTb
3+the stoichiometric ratio of each element takes MeO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder also mixes, wherein, and to be 0.01 ~ 0.06, MeO be in calcium oxide, strontium oxide and barium oxide one that x is 0.01 ~ 0.08, y.
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 oxygen, and the flow of working gas is 25sccm, and underlayer temperature is 500 DEG C.
Also comprise step: by described europium terbium codoped aluminium niobate light-emitting film vacuum annealing process 1h ~ 3h at 500 DEG C ~ 800 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 CaO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder is that 1mmol, 0.465mmol, 0.5mmol, 0.02mmol and 0.0075mmol mix according to mole number, and 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 oxygen is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C.The sample chemical formula obtained is CaAl
0.93nbO
5: 0.04Eu
3+, 0.03Tb
3+light-emitting film, be then 0.01Pa by the light-emitting film obtained vacuum tightness in vacuum tightness, annealing temperature is 600 DEG C, anneal 2h, then evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula of the europium terbium codoped aluminium niobate light-emitting film obtained in the present embodiment is CaAl
0.93nbO
5: 0.04Eu
3+, 0.03Tb
3+.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the europium terbium codoped aluminium niobate light-emitting film obtained.As seen from Figure 2, in electroluminescence spectrum, there is very strong glow peak in 490nm and 510nm wavelength zone, can be applied in thin-film electroluminescent displays.
Refer to Fig. 3, Fig. 3 is the XRD curve of europium terbium codoped aluminium niobate light-emitting film prepared by embodiment 1, test comparison standard P DF card.As can be seen from Figure 3, be the peak crystallization of aluminium calcium niobate, do 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 6.0V 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 88cd/m
2, show that device has the good characteristics of luminescence.
Embodiment 2
Select purity be 99.99% powder, by CaO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder is that 1mmol, 0.49mmol, 0.5mmol, 0.005mmol and 0.0025mmol mix according to mole number, and 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 oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 DEG C, and the chemical formula of the sample obtained is CaAl
0.98nbO
5: 0.01Eu
3+, 0.01Tb
3+light-emitting film, be then 0.01Pa by the light-emitting film obtained vacuum tightness in vacuum tightness, annealing temperature is 500 DEG C, anneal 1h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 3
Select purity be 99.99% powder, by CaO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder is that 1mmol, 0.43mmol, 0.5mmol, 0.04mmol and 0.015mmol mix according to mole number, and 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 oxygen is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, and the chemical formula of the sample obtained is CaAl
0.86nbO
5: 0.08Eu
3+, 0.06Tb
3+light-emitting film, be then 0.01Pa by the light-emitting film obtained vacuum tightness in vacuum tightness, annealing temperature is 800 DEG C, anneal 3h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 4
Select purity be 99.99% powder, by SrO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder is that 1mmol, 0.465mmol, 0.5mmol, 0.02mmol and 0.0075mmol mix according to mole number, and 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 oxygen is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C, and the chemical formula of the sample obtained is SrAl
0.93nbO
5: 0.04Eu
3+, 0.03Tb
3+light-emitting film, be then 0.01Pa by the light-emitting film obtained vacuum tightness in vacuum tightness, annealing temperature is 600 DEG C, anneal 2h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 5
Select purity be 99.99% powder, by SrO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder is that 1mmol, 0.49mmol, 0.5mmol, 0.005mmol and 0.0025mmol mix according to mole number, and 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 oxygen is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 DEG C.The chemical formula of the sample obtained is SrAl
0.98nbO
5: 0.01Eu
3+, 0.01Tb
3+light-emitting film, be then 0.01Pa by the light-emitting film obtained vacuum tightness in vacuum tightness, annealing temperature is 500 DEG C, anneal 1h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 6
Select purity be 99.99% powder, by SrO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder is that 1mmol, 0.43mmol, 0.5mmol, 0.04mmol and 0.015mmol mix according to mole number, and 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 oxygen is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, and the chemical formula of the sample obtained is SrAl
0.86nbO
5: 0.08Eu
3+, 0.06Tb
3+light-emitting film, be then 0.01Pa by the light-emitting film obtained vacuum tightness in vacuum tightness, annealing temperature is 800 DEG C, anneal 3h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 7
Select purity be 99.99% powder, by BaO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder is that 1mmol, 0.465mmol, 0.5mmol, 0.02mmol and 0.0075mmol mix according to mole number, and 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 oxygen is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C, and the chemical formula of the sample obtained is BaAl
0.93nbO
5: 0.04Eu
3+, 0.03Tb
3+light-emitting film, be then 0.01Pa by the light-emitting film obtained vacuum tightness in vacuum tightness, annealing temperature is 600 DEG C, anneal 2h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 8
Select purity be 99.99% powder, by BaO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder is that 1mmol, 0.49mmol, 0.5mmol, 0.005mmol and 0.0025mmol mix according to mole number, and 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 oxygen is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 DEG C.The chemical formula of the sample obtained is BaAl
0.98nbO
5: 0.01Eu
3+, 0.01Tb
3+light-emitting film, be then 0.01Pa by the light-emitting film obtained vacuum tightness in vacuum tightness, annealing temperature is 500 DEG C, anneal 1h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 9
Select purity be 99.99% powder, by BaO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder is that 1mmol, 0.43mmol, 0.5mmol, 0.04mmol and 0.015mmol mix according to mole number, and 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 oxygen is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, and the chemical formula of the sample obtained is BaAl
0.86nbO
5: 0.08Eu
3+, 0.06Tb
3+light-emitting film, be then 0.01Pa by the light-emitting film obtained vacuum tightness in vacuum tightness, annealing temperature is 800 DEG C, anneal 3h, 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 (10)
1. an europium terbium codoped aluminium niobate luminescent material, is characterized in that: its chemical formula is MeAl1
-x-ynbO
5: xEu
3+, yTb
3+, MeAl
1-x-ynbO
5matrix, Eu
3+and Tb
3+ion is active element, wherein, and to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y.
2. luminescent material according to claim 1, is characterized in that: described x is 0.04, y is 0.03.
3. a preparation method for europium terbium codoped aluminium niobate luminescent material, is characterized in that, comprise the following steps:
According to MeAl
1-x-ynbO
5: xEu
3+, yTb
3+the stoichiometric ratio of each element takes MeO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder also mixes, wherein, and to be 0.01 ~ 0.06, MeO be in calcium oxide, strontium oxide and barium oxide one that x is 0.01 ~ 0.08, y; And
Namely the powder mixed sinter 0.5 hour ~ 5 hours to be obtained chemical formula being MeAl at 900 DEG C ~ 1300 DEG C
1-x-ynbO
5: xEu
3+, yTb
3+europium terbium codoped aluminium niobate luminescent material, to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y.
4. an europium terbium codoped aluminium niobate light-emitting film, is characterized in that, the chemical general formula of the material of this europium terbium codoped aluminium niobate light-emitting film is MeAl
1-x-ynbO
5: xEu
3+, yTb
3+, MeAl
1-x-ynbO
5matrix, Eu
3+and Tb
3+ion is active element, wherein, and to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y.
5. a preparation method for europium terbium codoped aluminium niobate light-emitting film, is characterized in that, comprise the following steps:
According to MeAl
1-x-ynbO
5: xEu
3+, yTb
3+the stoichiometric ratio of each element takes MeO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder also mixes, and the powder mixed is sintered 0.5 hour ~ 5 hours at 900 DEG C ~ 1300 DEG C and obtains target, wherein, and to be 0.01 ~ 0.06, MeO be in calcium oxide, strontium oxide and barium oxide one that x is 0.01 ~ 0.08, y;
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 MeAl
1-x-ynbO
5: xEu
3+, yTb
3+europium terbium codoped aluminium niobate light-emitting film, to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y.
6. the preparation method of europium terbium codoped aluminium niobate light-emitting film according to claim 5, is characterized in that, also comprise step: by described europium terbium codoped aluminium niobate light-emitting film vacuum annealing process 1h ~ 3h at 500 DEG C ~ 800 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 europium terbium codoped aluminium niobate luminescent material, and the chemical formula of this europium terbium codoped aluminium niobate luminescent material is MeAl
1-x-ynbO
5: xEu
3+, yTb
3+, MeAl
1-x-ynbO
5matrix, Eu
3+and Tb
3+ion is active element, wherein, and to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y.
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 europium terbium codoped aluminium niobate luminescent material, and the chemical formula of this europium terbium codoped aluminium niobate luminescent material is MeAl1-x-yNbO
5: xEu
3+, yTb
3+, MeAl
1-x-ynbO
5matrix, Eu
3+and Tb
3+ion is active element, wherein, and to be 0.01 ~ 0.06, Me be in calcium constituent, strontium element and barium element one that x is 0.01 ~ 0.08, y;
Form negative electrode on the light-emitting 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 MeAl
1-x-ynbO
5: xEu
3+, yTb
3+the stoichiometric ratio of each element takes MeO, Al
2o
3, Nb
2o
5, Eu
2o
3and Tb
4o
7powder also to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, wherein, and to be 0.01 ~ 0.06, MeO be in calcium oxide, strontium oxide and barium oxide one that x is 0.01 ~ 0.08, y;
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.
10. the preparation method of membrane electro luminescent device according to claim 8, is characterized in that, also comprises step: by described europium terbium codoped aluminium niobate light-emitting film vacuum annealing process 1h ~ 3h at 500 DEG C ~ 800 DEG C.
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|---|---|---|---|---|
| CN110041929A (en) * | 2019-04-28 | 2019-07-23 | 上海应用技术大学 | A kind of oxide-base red fluorescence powder and preparation method thereof without rare earth |
-
2013
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110041929A (en) * | 2019-04-28 | 2019-07-23 | 上海应用技术大学 | A kind of oxide-base red fluorescence powder and preparation method thereof without rare earth |
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