CN104650890A - Samarium-doped gallium antimonate luminescent material, preparation method and application thereof - Google Patents

Samarium-doped gallium antimonate luminescent material, preparation method and application thereof Download PDF

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CN104650890A
CN104650890A CN201310578636.XA CN201310578636A CN104650890A CN 104650890 A CN104650890 A CN 104650890A CN 201310578636 A CN201310578636 A CN 201310578636A CN 104650890 A CN104650890 A CN 104650890A
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stibnate
sbo
xsm
samarium doping
doping gallium
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周明杰
陈吉星
王平
黄辉
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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

The invention relates to a samarium-doped gallium antimonate luminescent material, which comprises a following general chemical formula of Me5Ga1-xSbO9: xSm<3+>, wherein x is 0.01-0.05, Me is selected from at least one of magnesium element, calcium element, strontium element and barium element. In a photoluminescence spectrum of the samarium-doped gallium antimonate luminescent material, strong luminescence peaks of the samarium-doped gallium antimonate luminescent material are generated at 638nm and 727nm, the samarium-doped gallium antimonate luminescent material can be used in a thin-film electroluminescence display, and the invention also provides a preparation method and an application of the samarium-doped gallium antimonate luminescent material.

Description

Samarium doping gallium stibnate luminescent material, preparation method and application thereof
[technical field]
The present invention relates to a kind of samarium doping gallium stibnate luminescent material, its preparation method, samarium doping gallium stibnate 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 samarium doping gallium stibnate 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 samarium doping gallium stibnate luminescent material, its preparation method, samarium doping gallium stibnate light-emitting film, its preparation method, the membrane electro luminescent device using this samarium doping gallium stibnate luminescent material and preparation method thereof that can be applicable to membrane electro luminescent device.
A kind of samarium doping gallium stibnate luminescent material, its chemical formula is Me 5ga 1-xsbO 9: xSm 3+, wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
A preparation method for samarium doping gallium stibnate luminescent material, comprises the following steps:
According to Me 5ga 1-xsbO 9: xSm 3+the stoichiometric ratio of each element takes MeO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder also mixes, and wherein, x is that 0.01 ~ 0.05, MeO is selected from magnesium oxide, calcium oxide, at least one in strontium oxide and barium oxide; And
Namely the powder mixed sinter 0.5 hour ~ 5 hours to be obtained chemical formula being Me at 900 DEG C ~ 1300 DEG C 5ga 1-xsbO 9: xSm 3+samarium doping gallium stibnate luminescent material, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
A kind of samarium doping gallium stibnate light-emitting film, the chemical general formula of the material of this samarium doping gallium stibnate light-emitting film is Me 5ga 1-xsbO 9: xSm 3+, wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
A preparation method for samarium doping gallium stibnate light-emitting film, comprises the following steps:
According to Me 5ga 1-xsbO 9: xSm 3+the stoichiometric ratio of each element takes MeO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder also to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, and wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium oxide, calcium oxide, at least one in strontium oxide and barium oxide;
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 ~ 40sccm, underlayer temperature is 250 DEG C ~ 750 DEG C, laser energy is 80MJ ~ 300MJ, is then filmed, and obtaining chemical formula is Me 5ga 1-xsbO 9: xSm 3+samarium doping gallium stibnate light-emitting film, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
The preparation method of described samarium doping gallium stibnate 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 2.0Pa, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 DEG C, and laser energy is 150MJ.
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 samarium doping gallium stibnate luminescent material, and the chemical formula of this samarium doping gallium stibnate luminescent material is Me 5ga 1-xsbO 9: xSm 3+, wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
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 samarium doping gallium stibnate luminescent material, and the chemical formula of this samarium doping gallium stibnate luminescent material is Me 5ga 1-xsbO 9: xSm 3+, wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element;
Form negative electrode on the light-emitting layer.
The preparation of described luminescent layer comprises the following steps:
According to Me 5ga 1-xsbO 9: xSm 3+the stoichiometric ratio of each element takes MeO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder also to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, and wherein, x is that 0.01 ~ 0.05, MeO is selected from magnesium oxide, calcium oxide, at least one in strontium oxide and barium oxide;
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, and the flow of working gas is 10sccm ~ 40sccm, underlayer temperature is 250 DEG C ~ 750 DEG C, laser energy is 80MJ ~ 300MJ, is then filmed, and obtaining chemical formula is Me 5ga 1-xsbO 9: xSm 3+samarium doping gallium stibnate light-emitting film, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, and at least one in strontium element and barium element, described anode forms luminescent layer.
Described x is 0.02.
Above-mentioned samarium doping gallium stibnate luminescent material (Me 5ga 1-xsbO 9: xSm 3+) in the electroluminescent spectrum (EL) of light-emitting film made, have very strong glow peak in 638nm and 727nm 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 samarium doping gallium stibnate light-emitting film prepared by embodiment 1;
Fig. 3 is the XRD figure of samarium doping gallium stibnate 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, samarium doping gallium stibnate luminescent material, its preparation method, samarium doping gallium stibnate light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof are illustrated further.
The samarium doping gallium stibnate luminescent material of one embodiment, its chemical formula is Me 5ga 1-xsbO 9: xSm 3+, wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
Preferably, x is 0.02.
Me in this samarium doping gallium stibnate luminescent material 5ga 1-xsbO 9matrix, Sm 3+ion-activated element.In the electroluminescent spectrum (EL) of the light-emitting film that this samarium doping gallium stibnate luminescent material is made, there is very strong glow peak in 638nm and 727nm wavelength zone, can be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned samarium doping gallium stibnate luminescent material, comprises the following steps:
Step S11, according to Me 5ga 1-xsbO 9: xSm 3+the stoichiometric ratio of each element takes MeO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder also mixes, and wherein, x is that 0.01 ~ 0.05, MeO is selected from magnesium oxide, calcium oxide, at least one in strontium oxide and barium oxide.
In this step, preferably, x is 0.02.
Step S12, the equal powder of mixing is sintered 0.5 hour ~ 5 hours and can obtain samarium doping gallium stibnate luminescent material at 900 DEG C ~ 1300 DEG C, its chemical formula is Me 5ga 1-xsbO 9: xSm 3+, wherein, wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
In this step, preferably at 1250 DEG C, sinter 3 hours.
The samarium doping gallium stibnate light-emitting film of one embodiment, the chemical general formula of the material of this samarium doping gallium stibnate light-emitting film is Me 5ga 1-xsbO 9: xSm 3+samarium doping gallium stibnate luminescent material, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
Preferably, x is 0.02.
The preparation method of above-mentioned samarium doping gallium stibnate light-emitting film, comprises the following steps:
Step S21, by Me 5ga 1-xsbO 9: xSm 3+the stoichiometric ratio of each element takes MeO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder also to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, and wherein, x is 0.01 ~ 0.05.
In this step, preferably, x is 0.02, and at 1250 DEG C, sinter 3 hours become diameter to be 50mm, thickness is the ceramic target of 2mm.
Step S22, the target that obtains in step S21 and substrate are loaded the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 × 10 -3pa ~ 1.0 × 10 -5pa.
In this step, preferably, vacuum tightness is 5 × 10 -4pa.
Step S23, adjustment magnetron sputtering plating processing parameter are: base target spacing is 45mm ~ 95mm, magnetron sputtering operating pressure 0.2Pa ~ 4Pa, and the flow of working gas is 10sccm ~ 40sccm, and underlayer temperature is 250 DEG C ~ 750 DEG C; Laser energy is 80MJ ~ 300MJ, is then filmed, and obtaining chemical formula is Me 5ga 1-xsbO 9: xSm 3+samarium doping gallium stibnate light-emitting film, MeO is selected from magnesium oxide, calcium oxide, at least one in strontium oxide and barium oxide.
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 DEG C, and laser energy is 150MJ.
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 samarium doping gallium stibnate luminescent material, and the chemical formula of this samarium doping gallium stibnate luminescent material is Me 5ga 1-xsbO 9: xSm 3+, wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.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 samarium doping gallium stibnate luminescent material, and the chemical formula of this samarium doping gallium stibnate luminescent material is Me 5ga 1-xsbO 9: xSm 3+, wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
In present embodiment, luminescent layer 3 is obtained by following steps:
First, according to Me 5ga 1-xsbO 9: xSm 3+the stoichiometric ratio of each element takes MeO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder also to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, and wherein, x is that 0.01 ~ 0.05, MeO is selected from magnesium oxide, calcium oxide, at least one in strontium oxide and barium oxide.
In this step, preferably, x is 0.02, and at 1250 DEG C, sinter 3 hours become diameter to be 50mm, thickness is the ceramic target of 2mm.
Secondly, target and substrate are loaded the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 × 10 -3pa ~ 1.0 × 10 -5pa.
In this step, preferably, vacuum tightness is 5 × 10 -4pa.
Then, 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 ~ 40sccm, underlayer temperature is 250 DEG C ~ 750 DEG C, laser energy is 80MJ ~ 300MJ, is then filmed, and anode 2 is formed luminescent layer 3.
In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 2.0Pa, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 DEG C, and laser energy is 150MJ.
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 MgO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder is 10:0.98:1:0.02 according to mol ratio, 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 20sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 500 DEG C, laser energy 100MJ.The sample chemical formula obtained is Mg 5ga 0.98sbO 9: 0.02Sm 3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula of the samarium doping gallium stibnate light-emitting film obtained in the present embodiment is Mg 5ga 0.98sbO 9: 0.02Sm 3+, wherein Mg 5ga 0.98sbO 9matrix, Sm 3+it is active element.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the samarium doping gallium stibnate light-emitting film obtained.As seen from Figure 2, in electroluminescence spectrum, there is very strong glow peak in 638nm and 727nm wavelength zone, can be applied in thin-film electroluminescent displays.
Refer to Fig. 3, Fig. 3 is the XRD curve of samarium doping gallium stibnate 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 gallium stibnate, 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 80cd/m 2, show that device has the good characteristics of luminescence.
Embodiment 2
Select purity be 99.99% powder, by MgO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder is 10:0.95:1:0.05 according to mol ratio, 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, laser energy 80MJ.The chemical formula of the sample obtained is Mg 5ga 0.95sbO 9: 0.05Sm 3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 3
Select purity be 99.99% powder, by MgO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder is 10:0.99:1:0.01 according to mol ratio, 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 40sccm, and pressure is adjusted to 5.0Pa, and underlayer temperature is 750 DEG C, laser energy 300MJ.The chemical formula of the sample obtained is Mg 5ga 0.99sbO 9: 0.01Sm 3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 4
Select purity be 99.99% powder, by CaO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder is 10:0.98:1:0.02 according to mol ratio, 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 20sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 500 DEG C, laser energy 150MJ.The chemical formula of the sample obtained is Ca 5ga 0.98sbO 9: 0.02Sm 3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 5
Select purity be 99.99% powder, by CaO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder is 10:0.95:1:0.05 according to mol ratio, 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, laser energy 80MJ.The chemical formula of the sample obtained is Ca 5ga 0.95sbO 9: 0.05Sm 3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 6
Select purity be 99.99% powder, by CaO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder is 10:0.99:1:0.01 according to mol ratio, 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 40sccm, and pressure is adjusted to 5.0Pa, and underlayer temperature is 750 DEG C, laser energy 300MJ.The chemical formula of the sample obtained is Ca 5ga 0.99sbO 9: 0.01Sm 3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 7
Select purity be 99.99% powder, by SrO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder is 10:0.98:1:0.02 according to mol ratio, 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 20sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 500 DEG C, laser energy 150MJ.The chemical formula of the sample obtained is Sr 5ga 0.98sbO 9: 0.02Sm 3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 8
Select purity be 99.99% powder, by SrO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder is 10:0.95:1:0.05 according to mol ratio, 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, laser energy 80MJ.The chemical formula of the sample obtained is Sr 5ga 0.95sbO 9: 0.05Sm 3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 9
Select purity be 99.99% powder, by SrO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder is 10:0.99:1:0.01 according to mol ratio, 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 40sccm, and pressure is adjusted to 5.0Pa, and underlayer temperature is 750 DEG C, laser energy 300MJ.The chemical formula of the sample obtained is Sr 5ga 0.99sbO 9: 0.01Sm 3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 10
Select purity be 99.99% powder, by BaO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder is 10:0.98:1:0.02 according to mol ratio, 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 20sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 500 DEG C, laser energy 150MJ.The chemical formula of the sample obtained is Ba 5ga 0.98sbO 9: 0.02Sm 3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 11
Select purity be 99.99% powder, by BaO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder is 10:0.95:1:0.05 according to mol ratio, 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, laser energy 80MJ.The chemical formula of the sample obtained is Ba 5ga 0.95sbO 9: 0.05Sm 3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 12
Select purity be 99.99% powder, by BaO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder is 10:0.99:1:0.01 according to mol ratio, 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 40sccm, and pressure is adjusted to 5.0Pa, and underlayer temperature is 750 DEG C, laser energy 300MJ.The chemical formula of the sample obtained is Ba 5ga 0.99sbO 9: 0.01Sm 3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.

Claims (9)

1. a samarium doping gallium stibnate luminescent material, is characterized in that: its chemical formula is Me 5ga 1-xsbO 9: xSm 3+, wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
2. a preparation method for samarium doping gallium stibnate luminescent material, is characterized in that, comprise the following steps:
According to Me 5ga 1-xsbO 9: xSm 3+the stoichiometric ratio of each element takes MeO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder also mixes, and wherein, x is that 0.01 ~ 0.05, MeO is selected from magnesium oxide, calcium oxide, at least one in strontium oxide and barium oxide; And
Namely the powder mixed sinter 0.5 hour ~ 5 hours to be obtained chemical formula being Me at 900 DEG C ~ 1300 DEG C 5ga 1-xsbO 9: xSm 3+samarium doping gallium stibnate luminescent material, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
3. a samarium doping gallium stibnate light-emitting film, is characterized in that, the chemical general formula of the material of this samarium doping gallium stibnate light-emitting film is Me 5ga 1-xsbO 9: xSm 3+, wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
4. a preparation method for samarium doping gallium stibnate light-emitting film, is characterized in that, comprise the following steps:
According to Me 5ga 1-xsbO 9: xSm 3+the stoichiometric ratio of each element takes MeO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder also to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, and wherein, x is that 0.01 ~ 0.05, MeO is selected from magnesium oxide, calcium oxide, at least one in strontium oxide and barium oxide;
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 ~ 40sccm, underlayer temperature is 250 DEG C ~ 750 DEG C, laser energy is 80MJ ~ 300MJ, is then filmed, and obtaining chemical formula is Me 5ga 1-xsbO 9: xSm 3+samarium doping gallium stibnate light-emitting film, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
5. the preparation method of samarium doping gallium stibnate 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 2.0Pa, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 DEG C, and laser energy is 150MJ.
6. 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 samarium doping gallium stibnate luminescent material, and the chemical formula of this samarium doping gallium stibnate luminescent material is Me 5ga 1-xsbO 9: xSm 3+, wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element.
7. 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 samarium doping gallium stibnate luminescent material, and the chemical formula of this samarium doping gallium stibnate luminescent material is Me 5ga 1-xsbO 9: xSm 3+, wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, at least one in strontium element and barium element;
Form negative electrode on the light-emitting layer.
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 Me 5ga 1-xsbO 9: xSm 3+the stoichiometric ratio of each element takes MeO, Ga 2o 3, Sb 2o 5and Sm 2o 3powder also to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 hour ~ 5 hours, and wherein, x is that 0.01 ~ 0.05, Me is selected from magnesium oxide, calcium oxide, at least one in strontium oxide and barium oxide;
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, and the flow of working gas is 10sccm ~ 40sccm, underlayer temperature is 250 DEG C ~ 750 DEG C, laser energy is 80MJ ~ 300MJ, is then filmed, and obtaining chemical formula is Me 5ga 1-xsbO 9: xSm 3+samarium doping gallium stibnate light-emitting film, x is that 0.01 ~ 0.05, Me is selected from magnesium elements, calcium constituent, and at least one in strontium element and barium element, described anode forms luminescent layer.
9. the preparation method of membrane electro luminescent device according to claim 8, is characterized in that, described x is 0.02.
CN201310578636.XA 2013-11-18 2013-11-18 Samarium-doped gallium antimonate luminescent material, preparation method and application thereof Pending CN104650890A (en)

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