CN104178160A - Cerium terbium double-doped nitrogen silicon lanthanum luminescent material and preparation method and application thereof - Google Patents

Cerium terbium double-doped nitrogen silicon lanthanum luminescent material and preparation method and application thereof Download PDF

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CN104178160A
CN104178160A CN201310196485.1A CN201310196485A CN104178160A CN 104178160 A CN104178160 A CN 104178160A CN 201310196485 A CN201310196485 A CN 201310196485A CN 104178160 A CN104178160 A CN 104178160A
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codope
nitrogen silicon
cerium terbium
ytb
xce
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周明杰
王平
陈吉星
张娟娟
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

A cerium terbium double-doped nitrogen silicon lanthanum luminescent material has a chemical formula of La2Si6N10:xCe<3+>, yTb<3+>, wherein La2Si6N10 is a matrix, Ce<3+> and Tb<3+> are active elements, x is 0.01-0.05 and y is 0.01-0.06. In the electroluminescent spectra (EL) of a light-emitting film prepared by the cerium terbium double-doped nitrogen silicon lanthanum luminescent material, 490nm and 580nm wavelength regions both have strong light-emitting peaks, so that the light-emitting film can be used in a thin film electroluminescent display. The invention also provides a preparation method and application of the cerium terbium double-doped nitrogen silicon lanthanum luminescent material.

Description

Cerium terbium codope nitrogen silicon lanthanum luminescent material, preparation method and application thereof
[technical field]
The present invention relates to a kind of cerium terbium codope nitrogen silicon lanthanum luminescent material, its preparation method, cerium terbium codope nitrogen silicon lanthanum 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 luminous material of exploitation multiband, is the developing direction of this problem.But, can be applicable to the cerium terbium codope nitrogen silicon lanthanum 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 terbium codope nitrogen silicon lanthanum luminescent material, its preparation method, cerium terbium codope nitrogen silicon lanthanum light-emitting film, its preparation method that can be applicable to membrane electro luminescent device, use membrane electro luminescent device of this cerium terbium codope nitrogen silicon lanthanum luminescent material and preparation method thereof.
A cerium terbium codope nitrogen silicon lanthanum luminescent material, its chemical formula is La 2si 6n 10: xCe 3+, yTb 3+, La 2si 6n 10matrix, Ce 3+and Tb 3+ion is active element, and wherein, x is that 0.01~0.05, y is 0.01~0.06.
A preparation method for cerium terbium codope nitrogen silicon lanthanum luminescent material, comprises the following steps:
According to La 2si 6n 10: xCe 3+, yTb 3+the stoichiometric ratio of each element takes LaN, Si 3n 4, CeN and TbN powder also mix, and wherein, x is that 0.01~0.05, y is 0.01~0.06; And
The powder mixing sintering at 900 ℃~1300 ℃ is obtained to chemical formula for 0.5 hour~5 hours is La 2si 6n 10: xCe 3+, yTb 3+cerium terbium codope nitrogen silicon lanthanum luminescent material.
A cerium terbium codope nitrogen silicon lanthanum light-emitting film, the chemical general formula of the material of this cerium terbium codope nitrogen silicon lanthanum light-emitting film is La 2si 6n 10: xCe 3+, yTb 3+, wherein, x is that 0.01~0.05, y is 0.01~0.06.
A preparation method for cerium terbium codope nitrogen silicon lanthanum light-emitting film, comprises the following steps:
According to La 2si 6n 10: xCe 3+, yTb 3+the stoichiometric ratio of each element takes LaN, Si 3n 4, CeN and TbN powder also mix sintering at 900 ℃~1300 ℃ and make target in 0.5 hour~5 hours, and wherein, x is that 0.01~0.05, y is 0.01~0.06;
The vacuum cavity that described target and substrate is packed into magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10 -3pa~1.0 * 10 -5pa; And
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm~95mm, magnetron sputtering operating pressure 0.5Pa~5Pa, and the flow of working gas is 10sccm~40sccm, underlayer temperature is 250 ℃~750 ℃, laser energy is 80W~300W, is then filmed, and obtaining chemical formula is La 2si 6n 10: xCe 3+, yTb 3+cerium terbium codope nitrogen silicon lanthanum light-emitting film.
The vacuum tightness of described vacuum cavity is 5.0 * 10 -4pa, base target spacing is 60mm, and magnetron sputtering operating pressure is 3Pa, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃, and laser energy is 150W.
A kind of membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer stacking gradually, the material of described luminescent layer is cerium terbium codope nitrogen silicon lanthanum luminescent material, and the chemical formula of this cerium terbium codope nitrogen silicon lanthanum luminescent material is La 2si 6n 10: xCe 3+, yTb 3+, wherein, x is that 0.01~0.05, y is 0.01~0.06.
A preparation method for membrane electro luminescent device, comprises the following steps:
The substrate with anode is provided;
On described anode, form luminescent layer, the material of described luminescent layer is cerium terbium codope nitrogen silicon lanthanum luminescent material, and the chemical formula of this cerium terbium codope nitrogen silicon lanthanum luminescent material is La 2si 6n 10: xCe 3+, yTb 3+, wherein, x is that 0.01~0.05, y is 0.01~0.06;
On described luminescent layer, form negative electrode.
The preparation of described luminescent layer comprises the following steps:
According to La 2si 6n 10: xCe 3+, yTb 3+the stoichiometric ratio of each element takes LaN, Si 3n 4, CeN and TbN powder also mix sintering at 900 ℃~1300 ℃ and make target in 0.5 hour~5 hours, and wherein, x is that 0.01~0.05, y is 0.01~0.06;
The vacuum cavity that described target and described substrate is packed into magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10 -3pa~1.0 * 10 -5pa;
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm~95mm, magnetron sputtering operating pressure 0.5Pa~5Pa, and the flow of working gas is 10sccm~40sccm, underlayer temperature is 250 ℃~750 ℃, laser energy is 80W~300W, is then filmed, and obtaining chemical formula is La 2si 6n 10: xCe 3+, yTb 3+cerium terbium codope nitrogen silicon lanthanum light-emitting film, on described anode, form luminescent layer.
Above-mentioned cerium terbium codope nitrogen silicon lanthanum luminescent material (La 2si 6n 10: xCe 3+, yTb 3+) in the electroluminescent spectrum (EL) of the light-emitting film made, at 490nm and 580nm wavelength zone, there is very strong glow peak, 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 the cerium terbium codope nitrogen silicon lanthanum light-emitting film of embodiment 1 preparation;
Fig. 3 is the XRD figure of the cerium terbium codope nitrogen silicon lanthanum light-emitting film of 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 terbium codope nitrogen silicon lanthanum luminescent material, its preparation method, cerium terbium codope nitrogen silicon lanthanum light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof are further illustrated.
The cerium terbium codope nitrogen silicon lanthanum luminescent material of one embodiment, its chemical formula is La 2si 6n 10: xCe 3+, yTb 3+, La 2si 6n 10matrix, Ce 3+and Tb 3+ion is active element, and wherein, x is that 0.01~0.05, y is 0.01~0.06.
Preferably, x is that 0.02, y is 0.03.
La in this cerium terbium codope nitrogen silicon lanthanum luminescent material 2si 6n 10matrix, Ce 3+and Tb 3+ion is active element.In the electroluminescent spectrum (EL) of the light-emitting film that this cerium terbium codope nitrogen silicon lanthanum luminescent material is made, at 490nm and 580nm wavelength zone, there is very strong glow peak, can be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned cerium terbium codope nitrogen silicon lanthanum luminescent material, comprises the following steps:
Step S11, according to La 2si 6n 10: xCe 3+, yTb 3+the stoichiometric ratio of each element takes LaN, Si 3n 4, CeN and TbN powder, wherein, x is that 0.01~0.05, y is 0.01~0.06.
In this step, preferred, x is that 0.02, y is 0.03.
In this step, preferred, LaN, Si 3n 4, the mol ratio of CeN and TbN powder is 2:2:(0.01~0.05): (0.01~0.06);
Step S12, by mixing equal powder sintering at 900 ℃~1300 ℃, within 0.5 hour~5 hours, can obtain cerium terbium codope nitrogen silicon lanthanum luminescent material, its chemical formula is La 2si 6n 10: xCe 3+, yTb 3+, wherein, x is that 0.01~0.05, y is 0.01~0.06.
In this step, preferred sintering 3 hours at 1250 ℃.
The cerium terbium codope nitrogen silicon lanthanum light-emitting film of one embodiment, the chemical general formula of the material of this cerium terbium codope nitrogen silicon lanthanum light-emitting film is La 2si 6n 10: xCe 3+, yTb 3+cerium terbium codope nitrogen silicon lanthanum luminescent material.
Preferably, x is that 0.02, y is 0.03.
The preparation method of above-mentioned cerium terbium codope nitrogen silicon lanthanum light-emitting film, comprises the following steps:
Step S21, press La 2si 6n 10: xCe 3+, yTb 3+the stoichiometric ratio of each element takes LaN, Si 3n 4, CeN and TbN powder also mix sintering at 900 ℃~1300 ℃ and make target in 0.5 hour~5 hours, and wherein, x is that 0.01~0.05, y is 0.01~0.06.
In this step, preferred, x is that 0.02, y is 0.03, and at 1250 ℃, 3 hours one-tenth diameters of sintering are 50mm, the ceramic target that thickness is 2mm.
Step S22, the target obtaining in step S21 and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10 -3pa~1.0 * 10 -5pa.
In this step, preferred, vacuum tightness is 5 * 10 -4pa.
Step S23, adjustment magnetron sputtering plating processing parameter are: base target spacing is 45mm~95mm, magnetron sputtering operating pressure 0.5Pa~5Pa, and the flow of working gas is 10sccm~40sccm, underlayer temperature is 250 ℃~750 ℃; Laser energy is 80W~300W, is then filmed, and obtaining chemical formula is La 2si 6n 10: xCe 3+, yTb 3+cerium terbium codope nitrogen silicon lanthanum light-emitting film.
In this step, preferred, the vacuum tightness of vacuum cavity is 5.0 * 10 -4pa, base target spacing is 60mm, magnetron sputtering operating pressure 3Pa, working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃, and laser energy is 150W.
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 stacking 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 terbium codope nitrogen silicon lanthanum luminescent material, and the chemical formula of this cerium terbium codope nitrogen silicon lanthanum luminescent material is La 2si 6n 10: xCe 3+, yTb 3+, wherein, x is that 0.01~0.05, y is 0.01~0.06.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.The 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, on anode 2, form luminescent layer 3, the material of luminescent layer 3 is cerium terbium codope nitrogen silicon lanthanum luminescent material, and the chemical formula of this cerium terbium codope nitrogen silicon lanthanum luminescent material is La 2si 6n 10: xCe 3+, yTb 3+, wherein, x is that 0.01~0.05, y is 0.01~0.06.
In present embodiment, luminescent layer 3 is made by following steps:
First, by La 2si 6n 10: xCe 3+, yTb 3+the stoichiometric ratio of each element takes LaN, Si 3n 4, CeN and TbN powder also mix sintering at 900 ℃~1300 ℃ and make target in 0.5 hour~5 hours, and wherein, x is that 0.01~0.05, y is 0.01~0.06.
In this step, preferred, LaN, Si 3n 4, the mol ratio of CeN and TbN powder is 2:2:(0.01~0.05): (0.01~0.06);
In this step, preferred, x is that 0.02, y is 0.03, and at 1250 ℃, 3 hours one-tenth diameters of sintering are 50mm, the ceramic target that thickness is 2mm.
Secondly, target and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10 -3pa~1.0 * 10 -5pa.
In this step, preferred, vacuum tightness is 5 * 10 -4pa.
Then, adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm~95mm, magnetron sputtering operating pressure 0.5Pa~5Pa, the flow of working gas is 10sccm~40sccm, underlayer temperature is 250 ℃~750 ℃, laser energy is 80W~300W, is then filmed, and forms luminescent layer 3 on anode 2.
In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 3Pa, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃, and laser energy is 150W.
Step S33, on luminescent layer 3, form negative electrode 4.
In present embodiment, the material of negative electrode 4 is silver (Ag), by evaporation, is formed.
Be specific embodiment below.
Embodiment 1
Selecting purity is 99.99% powder, by LaN, and Si 3n 4, CeN and TbN powder according to mol ratio be 2:2:0.02:0.03 after even mixing, at 1250 ℃, sintering diameter 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 5.0 * 10 -4pa, the working gas flow of oxygen is 20sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 500 ℃, laser energy 150W.The sample chemical formula obtaining is La 2si 6n 10: 0.02Ce 3+, 0.03Tb 3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
The chemical general formula of the cerium terbium codope nitrogen silicon lanthanum light-emitting film obtaining in the present embodiment is La 2si 6n 10: 0.02Ce 3+, 0.03Tb 3+, La wherein 2si 6n 10matrix, Ce 3+and Tb 3+it is active element.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the cerium terbium codope nitrogen silicon lanthanum light-emitting film obtaining.As seen from Figure 2, in electroluminescence spectrum, at 490nm and 580nm wavelength zone, there is very strong glow peak, can be applied in thin-film electroluminescent displays.
Refer to Fig. 3, Fig. 3 is the XRD curve of the cerium terbium codope nitrogen silicon lanthanum light-emitting film of embodiment 1 preparation, test comparison standard P DF card.As can be seen from Figure 3, be the peak crystallization of nitrogen silicon lanthanum, there is not the diffraction peak of doped element and other impurity; Illustrate that the product that this preparation method obtains has good crystalline quality.
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 6.0V, curve 2 is voltage and brightness relationship curve, and the high-high brightness that can find out this device is 88cd/m 2, show that device has the good characteristics of luminescence.
Embodiment 2
Selecting purity is 99.99% powder, by LaN, and Si 3n 4, CeN and TbN powder according to mol ratio be 2:2:0.01:0.01 after even mixing, at 900 ℃, sintering diameter 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 1.0 * 10 -3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 ℃, laser energy 80W.The chemical formula of the sample obtaining is La 2si 6n 10: 0.01Ce 3+, 0.01Tb 3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 3
Selecting purity is 99.99% powder, by LaN, and Si 3n 4, CeN and TbN powder according to mol ratio be 2:2:0.05:0.06 after even mixing, at 1300 ℃, sintering diameter 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 1.0 * 10 -5pa, the working gas flow of oxygen is 40sccm, and pressure is adjusted to 5.0Pa, and underlayer temperature is 750 ℃, laser energy 300W.The chemical formula of the sample obtaining is La 2si 6n 10: 0.05Ce 3+, 0.06Tb 3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 4
Selecting purity is 99.99% powder, by LaN, and Si 3n 4, CeN and TbN powder according to mol ratio be 2:2:0.04:0.05 after even mixing, at 1250 ℃, sintering diameter 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 5.0 * 10 -4pa, the working gas flow of oxygen is 20sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 ℃, laser energy 300W.The chemical formula of the sample obtaining is La 2si 6n 10: 0.04Ce 3+, 0.05Tb 3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 5
Selecting purity is 99.99% powder, by LaN, and Si 3n 4, CeN and TbN powder according to mol ratio be 2:2:0.03:0.02 after even mixing, at 900 ℃, sintering diameter 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 1.0 * 10 -3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 ℃, laser energy 300W.The chemical formula of the sample obtaining is La 2si 6n 10: 0.03Ce 3+, 0.02Tb 3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 6
Selecting purity is 99.99% powder, by LaN, and Si 3n 4, CeN and TbN powder according to mol ratio be 2:2:0.02:0.04 after even mixing, at 1300 ℃, sintering diameter 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 1.0 * 10 -5pa, the working gas flow of oxygen is 40sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 ℃, laser energy 80W.The chemical formula of the sample obtaining is La 2si 6n 10: 0.02Ce 3+, 0.04Tb 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 (9)

1. a cerium terbium codope nitrogen silicon lanthanum luminescent material, is characterized in that: its chemical formula is La 2si 6n 10: xCe 3+, yTb 3+, La 2si 6n 10matrix, Ce 3+and Tb 3+ion is active element, and wherein, x is that 0.01~0.05, y is 0.01~0.06.
2. a preparation method for cerium terbium codope nitrogen silicon lanthanum luminescent material, is characterized in that, comprises the following steps:
According to La 2si 6n 10: xCe 3+, yTb 3+the stoichiometric ratio of each element takes LaN, Si 3n 4, CeN and TbN powder also mix, and wherein, x is that 0.01~0.05, y is 0.01~0.06; And
The powder mixing sintering at 900 ℃~1300 ℃ is obtained to chemical formula for 0.5 hour~5 hours is La 2si 6n 10: xCe 3+, yTb 3+cerium terbium codope nitrogen silicon lanthanum luminescent material.
3. a cerium terbium codope nitrogen silicon lanthanum light-emitting film, is characterized in that, the chemical general formula of the material of this cerium terbium codope nitrogen silicon lanthanum light-emitting film is La 2si 6n 10: xCe 3+, yTb 3+, wherein, x is that 0.01~0.05, y is 0.01~0.06.
4. a preparation method for cerium terbium codope nitrogen silicon lanthanum light-emitting film, is characterized in that, comprises the following steps:
According to La 2si 6n 10: xCe 3+, yTb 3+the stoichiometric ratio of each element takes LaN, Si 3n 4, CeN and TbN powder also mix sintering at 900 ℃~1300 ℃ and make target in 0.5 hour~5 hours, and wherein, x is that 0.01~0.05, y is 0.01~0.06;
The vacuum cavity that described target and substrate is packed into magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10 -3pa~1.0 * 10 -5pa; And
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm~95mm, magnetron sputtering operating pressure 0.5Pa~5Pa, and the flow of working gas is 10sccm~40sccm, underlayer temperature is 250 ℃~750 ℃, laser energy is 80W~300W, is then filmed, and obtaining chemical formula is La 2si 6n 10: xCe 3+, yTb 3+cerium terbium codope nitrogen silicon lanthanum light-emitting film.
5. the preparation method of cerium terbium codope nitrogen silicon lanthanum 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 3Pa, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃, and laser energy is 150W.
6. a membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer stacking gradually, it is characterized in that, the material of described luminescent layer is cerium terbium codope nitrogen silicon lanthanum luminescent material, and the chemical formula of this cerium terbium codope nitrogen silicon lanthanum luminescent material is La 2si 6n 10: xCe 3+, yTb 3+, wherein, x is that 0.01~0.05, y is 0.01~0.06.
7. a preparation method for membrane electro luminescent device, is characterized in that, comprises the following steps:
The substrate with anode is provided;
On described anode, form luminescent layer, the material of described luminescent layer is cerium terbium codope nitrogen silicon lanthanum luminescent material, and the chemical formula of this cerium terbium codope nitrogen silicon lanthanum luminescent material is La 2si 6n 10: xCe 3+, yTb 3+, wherein, x is that 0.01~0.05, y is 0.01~0.06;
On described luminescent layer, form negative electrode.
8. the preparation method of membrane electro luminescent device according to claim 7, is characterized in that, the preparation of described luminescent layer comprises the following steps:
According to La 2si 6n 10: xCe 3+, yTb 3+the stoichiometric ratio of each element takes LaN, Si 3n 4, CeN and TbN powder also mix sintering at 900 ℃~1300 ℃ and make target in 0.5 hour~5 hours, and wherein, x is that 0.01~0.05, y is 0.01~0.06;
The vacuum cavity that described target and described substrate is packed into magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10 -3pa~1.0 * 10 -5pa;
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm~95mm, magnetron sputtering operating pressure 0.5Pa~5Pa, and the flow of working gas is 10sccm~40sccm, underlayer temperature is 250 ℃~750 ℃, laser energy is 80W~300W, is then filmed, and obtaining chemical formula is La 2si 6n 10: xCe 3+, yTb 3+cerium terbium codope nitrogen silicon lanthanum light-emitting film, on described anode, form luminescent layer.
9. the preparation method of membrane electro luminescent device according to claim 8, is characterized in that, described x is that 0.02, y is 0.03.
CN201310196485.1A 2013-05-22 2013-05-22 Cerium terbium double-doped nitrogen silicon lanthanum luminescent material and preparation method and application thereof Pending CN104178160A (en)

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Application publication date: 20141203