CN103571468A - Antimony terbium co-doped silicon aluminum nitrogen oxide light-emitting material and preparation method and application thereof - Google Patents
Antimony terbium co-doped silicon aluminum nitrogen oxide light-emitting material and preparation method and application thereof Download PDFInfo
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- CN103571468A CN103571468A CN201210268400.1A CN201210268400A CN103571468A CN 103571468 A CN103571468 A CN 103571468A CN 201210268400 A CN201210268400 A CN 201210268400A CN 103571468 A CN103571468 A CN 103571468A
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Abstract
An antimony terbium co-doped silicon aluminum nitrogen oxide light-emitting material has a chemical formula of SiAlON: xSb<3+>, yTb<3+>, wherein SiAlON is a matrix, antimony ions and terbium ions are active elements, x is 0.01 ~ 0.05 and y is 0.01 ~ 0.08. In the electroluminescent spectra (EL) of a light-emitting film prepared by the antimony terbium co-doped silicon aluminum nitrogen oxide light-emitting material, strong light-emitting peaks at 490nm and 580nm wavelength regions exist, 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 antimony terbium co-doped silicon aluminum nitrogen oxide light-emitting material.
Description
Technical field
The present invention relates to a kind of antimony terbium codoped sial nitrogen oxides luminescent material, its preparation method, antimony terbium codoped sial oxynitrides 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 antimony terbium codoped sial nitrogen oxides 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 antimony terbium codoped sial nitrogen oxides luminescent material, its preparation method, antimony terbium codoped sial oxynitrides light-emitting film, its preparation method that can be applicable to membrane electro luminescent device, use membrane electro luminescent device of this antimony terbium codoped sial nitrogen oxides luminescent material and preparation method thereof.
A terbium codoped sial nitrogen oxides luminescent material, its chemical formula is SiAlON:xSb
3+, yTb
3+, wherein SiAlON is matrix, and antimony ion and terbium ion are active elements, and x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08.
In a preferred embodiment, x is that 0.02, y is 0.04.
A preparation method for antimony terbium codoped sial nitrogen oxides luminescent material, comprises the following steps:
According to SiAlON:xSb
3+, yTb
3+the stoichiometric ratio of each element takes Si
3n
4, Al
2o
3, SbO
2and Tb
4o
7powder also mixes, and wherein x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08; And
The powder mixing sintering at 900 ℃ ~ 1300 ℃ is obtained to chemical formula for 0.5 hour ~ 5 hours is SiAlON:xSb
3+, yTb
3+antimony terbium codoped sial nitrogen oxides luminescent material.
A terbium codoped sial oxynitrides light-emitting film, the chemical general formula of the material of this antimony terbium codoped sial oxynitrides light-emitting film is SiAlON:xSb
3+, yTb
3+, wherein, SiAlON is matrix, and antimony ion and terbium ion are active elements, and x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08.
A preparation method for antimony terbium codoped sial oxynitrides light-emitting film, comprises the following steps:
According to SiAlON:xSb
3+, yTb
3+the stoichiometric ratio of each element takes Si
3n
4, Al
2o
3, SbO
2and Tb
4o
7powder also mixes sintering at 900 ℃ ~ 1300 ℃ and within 0.5 hour ~ 5 hours, makes target, and wherein x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08;
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, the energy of laser is 80W ~ 300W, the flow of working gas is 10sccm ~ 40sccm, underlayer temperature is 250 ℃ ~ 750 ℃, then be filmed, obtaining chemical formula is SiAlON:xSb
3+, yTb
3+antimony terbium codoped sial oxynitrides light-emitting film.
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 3Pa, and the energy of laser is 150W, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃.
A kind of membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer stacking gradually, the material of described luminescent layer is antimony terbium codoped sial nitrogen oxides luminescent material, and the chemical formula of this antimony terbium codoped sial nitrogen oxides luminescent material is SiAlON:xSb
3+, yTb
3+, wherein SiAlON is matrix, and antimony ion and terbium ion are active elements, and x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08.
In a preferred embodiment, x is that 0.02, y is 0.04.
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 antimony terbium codoped sial nitrogen oxides luminescent material, and the chemical formula of this antimony terbium codoped sial nitrogen oxides luminescent material is SiAlON:xSb
3+, yTb
3+, wherein SiAlON is matrix, and antimony ion and terbium ion are active elements, and x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08;
On described luminescent layer, form negative electrode.
In a preferred embodiment, the preparation of described luminescent layer comprises the following steps:
According to SiAlON:xSb
3+, yTb
3+the stoichiometric ratio of each element takes Si
3n
4, Al
2o
3, SbO
2and Tb
4o
7powder also mixes sintering at 900 ℃ ~ 1300 ℃ and within 0.5 hour ~ 5 hours, makes target, and wherein x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08;
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, the energy of laser is 80W ~ 300W, the flow of working gas is 10sccm ~ 40sccm, underlayer temperature is 250 ℃ ~ 750 ℃, then be filmed, obtaining chemical formula is SiAlON:xSb
3+, yTb
3+antimony terbium codoped sial oxynitrides light-emitting film, on described anode, form luminescent layer.
Above-mentioned antimony terbium codoped sial nitrogen oxides luminescent material (SiAlON:xSb
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 antimony terbium codoped sial oxynitrides light-emitting film of embodiment 1 preparation;
Fig. 3 is the XRD figure of the antimony terbium codoped sial oxynitrides 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, antimony terbium codoped sial nitrogen oxides luminescent material, its preparation method, antimony terbium codoped sial oxynitrides light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof are further illustrated.
The antimony terbium codoped sial nitrogen oxides luminescent material of one embodiment, its chemical formula is SiAlON:xSb
3+, yTb
3+, wherein SiAlON is matrix, and antimony ion and terbium ion are active elements, and x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08.
Preferably, x is that 0.02, y is 0.04.
In this antimony terbium codoped sial nitrogen oxides luminescent material, SiAlON is matrix, and antimony ion and terbium ion are active elements.In the electroluminescent spectrum (EL) of the light-emitting film that this antimony terbium codoped sial nitrogen oxides 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 antimony terbium codoped sial nitrogen oxides luminescent material, comprises the following steps:
Step S11, according to SiAlON:xSb
3+, yTb
3+the stoichiometric ratio of each element takes Si
3n
4, Al
2o
3, SbO
2and Tb
4o
7powder, wherein x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08.
In this step, preferred, x is that 0.02, y is 0.04.
Step S12, by mixing equal powder sintering at 900 ℃ ~ 1300 ℃, within 0.5 hour ~ 5 hours, can obtain antimony terbium codoped sial nitrogen oxides luminescent material, its chemical formula is SiAlON:xSb
3+, yTb
3+, wherein SiAlON is matrix, and antimony ion and terbium ion are active elements, and x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08.
In this step, preferred sintering 3 hours at 1250 ℃.
The antimony terbium codoped sial oxynitrides light-emitting film of one embodiment, the chemical general formula of the material of this antimony terbium codoped sial oxynitrides light-emitting film is SiAlON:xSb
3+, yTb
3+, wherein, SiAlON is matrix, and antimony ion and terbium ion are active elements, and x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08.
Preferably, x is that 0.02, y is 0.04.
The preparation method of above-mentioned antimony terbium codoped sial oxynitrides light-emitting film, comprises the following steps:
Step S21, press SiAlON:xSb
3+, yTb
3+the stoichiometric ratio of each element takes Si
3n
4, Al
2o
3, SbO
2and Tb
4o
7powder also mixes sintering at 900 ℃ ~ 1300 ℃ and within 0.5 hour ~ 5 hours, makes target, and wherein x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08.
In this step, preferred, x is that 0.02, y is 0.04, 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 energy of laser is 80W ~ 300W, and the flow of working gas is 10sccm ~ 40sccm, and underlayer temperature is 250 ℃ ~ 750 ℃; Then be filmed, obtaining chemical formula is SiAlON:xSb
3+, yTb
3+antimony terbium codoped sial oxynitrides light-emitting film.
In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 3Pa, and the energy of laser is 150W, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃.
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 antimony terbium codoped sial nitrogen oxides luminescent material, and the chemical formula of this antimony terbium codoped sial nitrogen oxides luminescent material is SiAlON:xSb
3+, yTb
3+, wherein, SiAlON is matrix, and antimony ion and terbium ion are active elements, and x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08, and 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 antimony terbium codoped sial nitrogen oxides luminescent material, and the chemical formula of this antimony terbium codoped sial nitrogen oxides luminescent material is SiAlON:xSb
3+, yTb
3+, wherein, SiAlON is matrix, and antimony ion and terbium ion are active elements, and x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08.
In present embodiment, luminescent layer 3 is made by following steps:
First, by SiAlON:xSb
3+, yTb
3+the stoichiometric ratio of each element takes Si
3n
4, Al
2o
3, SbO
2and Tb
4o
7powder also mixes sintering at 900 ℃ ~ 1300 ℃ and within 0.5 hour ~ 5 hours, makes target, and wherein x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08.
In this step, preferred, x is that 0.02, y is 0.04, 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 energy of laser is 80W ~ 300W, the flow of working gas is 10sccm ~ 40sccm, underlayer temperature is 250 ℃ ~ 750 ℃, 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 the energy of laser is 150W, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃.
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, takes Al
2o
3, Si
3n
4, SbO
2and Tb
4o
7powder, its mol ratio is 0.84:0.1:0.02:0.04, 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 ℃, and laser energy is 150W.The sample chemical formula obtaining is SiAlON:0.02Sb
3+, 0.04Tb
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
The chemical general formula of the antimony terbium codoped sial oxynitrides light-emitting film obtaining in the present embodiment is SiAlON:0.02Sb
3+, 0.04Tb
3+, wherein SiAlON is matrix, Sb
3+and Tb
3+ion is active element.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the antimony terbium codoped sial oxynitrides 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 antimony terbium codoped sial oxynitrides light-emitting film of embodiment 1 preparation, test comparison standard P DF card.From Fig. 3, can all diffraction peaks be the crystalline characteristics peak that sial oxynitrides is corresponding, not occur doped element and the relevant diffraction peak of other impurity, interpret sample has good crystalline structure.
Refer to Fig. 4, Fig. 4 is the voltage of membrane electro luminescent device of embodiment 1 preparation and the graph of relation between current density and voltage and brightness, curve 1 is voltage and current density relation curve, can find out that this device starts luminous from voltage 5.0V, curve 2 is voltage and brightness relationship curve, and the high-high brightness that can find out this device is 83cd/m
2, show that device has the good characteristics of luminescence.
Embodiment 2
Selecting purity is 99.99% powder, takes Al
2o
3, Si
3n
4, SbO
2and Tb
4o
7powder, its mol ratio is 0.83:0.15:0.01:0.01, 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 ℃, and laser energy is 80W.The sample chemical formula obtaining is SiAlON:0.01Sb
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, takes Al
2o
3, Si
3n
4, SbO
2and Tb
4o
7powder, its mol ratio is 0.687:0.3:0.05:0.08, 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 argon gas is 40sccm, and pressure is adjusted to 5.0Pa, and underlayer temperature is 750 ℃, and laser energy is 300W.Obtaining chemical formula is SiAlON:0.05Sb
3+, 0.08Tb
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 4
Selecting purity is 99.99% powder, takes Al
2o
3, Si
3n
4, SbO
2and Tb
4o
7powder, its mol ratio is 0.796:0.2:0.02:0.02, 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 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 ℃, and laser energy is 300W.Obtaining chemical formula is SiAlON:0.02Sb
3+, 0.02Tb
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 5
Selecting purity is 99.99% powder, takes Al
2o
3, Si
3n
4, SbO
2and Tb
4o
7powder, its mol ratio is 0.67:0.25:0.03:0.05, 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 0.2Pa, and underlayer temperature is 250 ℃, and laser energy is 300W.Obtaining chemical formula is SiAlON:0.03Sb
3+, 0.05Tb
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Selecting purity is 99.99% powder, takes Al
2o
3, Si
3n
4, SbO
2and Tb
4o
7powder, its mol ratio is 0.8:0.1:0.04:0.06, 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 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 ℃, and laser energy is 300W.Obtaining chemical formula is SiAlON:0.04Sb
3+, 0.06Tb
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 7
Selecting purity is 99.99% powder, takes Al
2o
3, Si
3n
4, SbO
2and Tb
4o
7powder, its mol ratio is 0.6:0.3:0.03:0.07, 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 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 ℃, and laser energy is 300W.Obtaining chemical general formula is SiAlON:0.03Sb
3+, 0.07Tb
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. an antimony terbium codoped sial nitrogen oxides luminescent material, is characterized in that: its chemical formula is SiAlON:xSb
3+, yTb
3+, wherein SiAlON is matrix, and antimony ion and terbium ion are active elements, and x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08.
2. antimony terbium codoped sial nitrogen oxides luminescent material according to claim 1, is characterized in that: described x is that 0.02, y is 0.04.
3. a preparation method for antimony terbium codoped sial nitrogen oxides luminescent material, is characterized in that, comprises the following steps:
According to SiAlON:xSb
3+, yTb
3+the stoichiometric ratio of each element takes Si
3n
4, Al
2o
3, SbO
2and Tb
4o
7powder also mixes, and wherein, x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08; And
The powder mixing sintering at 900 ℃ ~ 1300 ℃ is obtained to chemical formula for 0.5 hour ~ 5 hours is SiAlON:xSb
3+, yTb
3+antimony terbium codoped sial nitrogen oxides luminescent material.
4. an antimony terbium codoped sial oxynitrides light-emitting film, is characterized in that, the chemical general formula of the material of this antimony terbium codoped sial oxynitrides light-emitting film is SiAlON:xSb
3+, yTb
3+, wherein SiAlON is matrix, and antimony ion and terbium ion are active elements, and x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08.
5. a preparation method for antimony terbium codoped sial oxynitrides light-emitting film, is characterized in that, comprises the following steps:
According to SiAlON:xSb
3+, yTb
3+the stoichiometric ratio of each element takes Si
3n
4, Al
2o
3, SbO
2and Tb
4o
7powder also mixes sintering at 900 ℃ ~ 1300 ℃ and makes target in 0.5 hour ~ 5 hours, and wherein, x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08;
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, the energy of laser is 80W ~ 300W, the flow of working gas is 10sccm ~ 40sccm, underlayer temperature is 250 ℃ ~ 750 ℃, then be filmed, obtaining chemical formula is SiAlON:xSb
3+, yTb
3+antimony terbium codoped sial oxynitrides light-emitting film.
6. the preparation method of antimony terbium codoped sial oxynitrides light-emitting film according to claim 5, 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 the energy of laser is 150W, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃.
7. a membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer stacking gradually, it is characterized in that, the material of described luminescent layer is antimony terbium codoped sial nitrogen oxides luminescent material, and the chemical formula of this antimony terbium codoped sial nitrogen oxides luminescent material is SiAlON:xSb
3+, yTb
3+, wherein SiAlON is matrix, and antimony ion and terbium ion are active elements, and x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08.
8. membrane electro luminescent device according to claim 7, is characterized in that, described x is that 0.02, y is 0.04.
9. 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 antimony terbium codoped sial nitrogen oxides luminescent material, and the chemical formula of this antimony terbium codoped sial nitrogen oxides luminescent material is SiAlON:xSb
3+, yTb
3+, wherein SiAlON is matrix, and antimony ion and terbium ion are active elements, and x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08;
On described luminescent layer, form negative electrode.
10. the preparation method of membrane electro luminescent device according to claim 9, is characterized in that, the preparation of described luminescent layer comprises the following steps:
According to SiAlON:xSb
3+, yTb
3+the stoichiometric ratio of each element takes Si
3n
4, Al
2o
3, SbO
2and Tb
4o
7powder also mixes sintering at 900 ℃ ~ 1300 ℃ and within 0.5 hour ~ 5 hours, makes target, and wherein x is that 0.01 ~ 0.05, y is 0.01 ~ 0.08;
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, the energy of laser is 80W ~ 300W, the flow of working gas is 10sccm ~ 40sccm, underlayer temperature is 250 ℃ ~ 750 ℃, then be filmed, obtaining chemical formula is SiAlON:xSb
3+, yTb
3+antimony terbium codoped sial oxynitrides light-emitting film, on described anode, form luminescent layer.
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CN106242583A (en) * | 2016-08-08 | 2016-12-21 | 屠秀芬 | The nano oxidized terbium of a kind of SiALON is combined the preparation method of magneto-optic crystalline ceramics |
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