CN104119864A - Samarium doped silicon nitride luminescent material and preparation method and application thereof - Google Patents
Samarium doped silicon nitride luminescent material and preparation method and application thereof Download PDFInfo
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- CN104119864A CN104119864A CN201310150177.5A CN201310150177A CN104119864A CN 104119864 A CN104119864 A CN 104119864A CN 201310150177 A CN201310150177 A CN 201310150177A CN 104119864 A CN104119864 A CN 104119864A
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- silicon nitride
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Abstract
The invention discloses a samarium doped silicon nitride luminescent material with a chemical formula of Me2Si5N8:xSm<3 +>, wherein Me2Si5N8 is a matrix, samarium ions are activating elements, x is 0.01-0.05, and Me is one of zinc, magnesium, calcium, strontium and barium elements. The electroluminescent spectra (EL) of a luminescent film prepared from the samarium doped silicon nitride luminescent material has very strong luminescence peaks in 638 nm and 727 nm wavelength regions, and the luminescent film can be applied to film electroluminescent displays. The invention also provides a preparation method and application of the samarium doped silicon nitride luminescent material.
Description
[technical field]
The present invention relates to a kind of samarium doped silicon nitride luminescent material, its preparation method, samarium doped silicon nitride 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 samarium doped silicon nitride 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 samarium doped silicon nitride luminescent material that can be applicable to membrane electro luminescent device, its preparation method, samarium doped silicon nitride light-emitting film, its preparation method, the membrane electro luminescent device that uses this samarium doped silicon nitride luminescent material and preparation method thereof.
A kind of samarium doped silicon nitride luminescent material, its chemical formula is Me
2si
5n
8: xSm
3+, wherein Me
2si
5n
8be matrix, samarium ion is active element, and x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
A preparation method for samarium doped silicon nitride luminescent material, comprises the following steps:
According to Me
2si
5n
8: xSm
3+the stoichiometric ratio of each element takes Me
3n
2, Si
3n
4with SmN powder and mix, wherein, x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element; And
The powder mixing sintering at 900 DEG C～1300 DEG C is obtained to chemical formula for 0.5 hour～5 hours is Me
2si
5n
8: xSm
3+samarium doped silicon nitride luminescent material.
A kind of samarium doped silicon nitride light-emitting film, the chemical general formula of the material of this samarium doped silicon nitride light-emitting film is Me
2si
5n
8: xSm
3+, wherein Me
2si
5n
8be matrix, samarium ion is active element, and x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
A preparation method for samarium doped silicon nitride light-emitting film, comprises the following steps:
According to Me
2si
5n
8: xSm
3+the stoichiometric ratio of each element takes Me
3n
2, Si
3n
4with SmN powder and mix sintering at 900 DEG C～1300 DEG C and make target in 0.5 hour～5 hours, wherein, x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element;
Described 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; And
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C, sputtering power 80～300W, is then filmed, and obtaining chemical formula is Me
2si
5n
8: xSm
3+samarium doped silicon nitride light-emitting film.
Described Me
3n
2, Si
3n
4with the mol ratio of SmN powder be 2:5:(0.03～0.15).
The vacuum tightness of described vacuum cavity is 5.0 × 10
-4pa, base target spacing is 60mm, and magnetron sputtering operating pressure is 2Pa, and working gas is oxygen, and the flow of working gas is 25sccm, underlayer temperature is 500 DEG C, sputtering power 100W.
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, and the material of described luminescent layer is samarium doped silicon nitride luminescent material, and the chemical formula of this samarium doped silicon nitride luminescent material is Me
2si
5n
8: xSm
3+, wherein Me
2si
5n
8be matrix, samarium ion is active element, and x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
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 samarium doped silicon nitride luminescent material, and the chemical formula of this samarium doped silicon nitride luminescent material is Me
2si
5n
8: xSm
3+, wherein Me
2si
5n
8be matrix, samarium ion is active element, and x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element;
On described luminescent layer, form negative electrode.
In a preferred embodiment, the preparation of described luminescent layer comprises the following steps:
According to Me
2si
5n
8: xSm
3+the stoichiometric ratio of each element takes Me
3n
2, Si
3n
4with SmN powder and mix sintering at 900 DEG C～1300 DEG C and within 0.5 hour～5 hours, make target, wherein x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element;
Described target and described 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;
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C, sputtering power 80～300W, then be filmed, on described anode, form luminescent layer.
Described Me
3n
2, Si
3n
4with the mol ratio of SmN powder be 2:5:(0.03～0.15).
Above-mentioned samarium doped silicon nitride luminescent material (Me
2si
5n
8: xSm
3+) in the electroluminescent spectrum (EL) of the light-emitting film made, there is very strong glow peak at 638nm and 727nm wavelength zone, can be applied in thin-film electroluminescent displays.
[brief description of the drawings]
Fig. 1 is the structural representation of the membrane electro luminescent device of an embodiment;
Fig. 2 is the electroluminescent spectrogram of the samarium doped silicon nitride light-emitting film prepared of embodiment 1;
Fig. 3 is the XRD figure of the samarium doped silicon nitride light-emitting film prepared of embodiment 1;
Fig. 4 is the graph of relation between voltage and current density and voltage and the brightness of the membrane electro luminescent device prepared of embodiment 1.
[embodiment]
Below in conjunction with the drawings and specific embodiments, samarium doped silicon nitride luminescent material, its preparation method, samarium doped silicon nitride light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof are further illustrated.
The samarium doped silicon nitride luminescent material of one embodiment, its chemical formula is Me
2si
5n
8: xSm
3+, wherein Me
2si
5n
8be matrix, samarium ion is active element, and x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
Preferably, x is 0.03.
Me in this samarium doped silicon nitride luminescent material
2si
5n
8be matrix, samarium ion is active element.In the electroluminescent spectrum (EL) of the light-emitting film that this samarium doped silicon nitride luminescent material is made, there is very strong glow peak at 638nm and 727nm wavelength zone, can be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned samarium doped silicon nitride luminescent material, comprises the following steps:
Step S11, according to Me
2si
5n
8: xSm
3+the stoichiometric ratio of each element takes Me
3n
2, Si
3n
4with SmN powder and mix, wherein, x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
In this step, preferred, x is 0.03.
Step S12, the powder mixing sintering at 900 DEG C～1300 DEG C can be obtained to samarium doped silicon nitride luminescent material in 0.5 hour～5 hours, its chemical formula is Me
2si
5n
8: xSm
3+samarium doped silicon nitride.
In this step, preferably sintering 3 hours at 1250 DEG C.
The samarium doped silicon nitride light-emitting film of one embodiment, the chemical general formula of this samarium doped silicon nitride light-emitting film is Me
2si
5n
8: xSm
3+, wherein Me
2si
5n
8be matrix, samarium ion is active element, and x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
Preferably, x is 0.03.
The preparation method of above-mentioned samarium doped silicon nitride light-emitting film, comprises the following steps:
Step S21, press Me
2si
5n
8: xSm
3+the stoichiometric ratio of each element takes Me
3n
2, Si
3n
4with SmN powder and mix sintering at 900 DEG C～1300 DEG C and make target in 0.5 hour～5 hours, wherein, x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
In this step, preferred, x is 0.03, and at 1250 DEG C, 3 hours one-tenth diameters of sintering are 50mm, the ceramic target that thickness is 2mm.
In this step, preferred, described Me
3n
2, Si
3n
4with the mol ratio of SmN powder be 2:5:(0.03～0.15).
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 0.2Pa～4Pa, the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C, sputtering power 80～300W, then be filmed, obtaining chemical formula is Me
2si
5n
8: xSm
3+samarium doped silicon nitride light-emitting film.
In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 2Pa, and working gas is oxygen, and the flow of working gas is 25sccm, and underlayer temperature is 500 DEG C, sputtering power 100W.
Refer to Fig. 1, the membrane electro luminescent device 100 of an embodiment, this membrane electro luminescent device 100 comprises the substrate 1, anode 2, luminescent layer 3 and the negative electrode 4 that stack gradually.
Substrate 1 is glass substrate.Anode 2 is for being formed at the tin indium oxide (ITO) in glass substrate.The material of luminescent layer 3 is samarium doped silicon nitride luminescent material, and the chemical formula of this samarium doped silicon nitride luminescent material is Me
2si
5n
8: xSm
3+, wherein Me
2si
5n
8be matrix, samarium ion is active element, and x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, 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.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 samarium doped silicon nitride luminescent material, and the chemical formula of this samarium doped silicon nitride luminescent material is Me
2si
5n
8: xSm
3+, wherein Me
2si
5n
8be matrix, samarium ion is active element, and x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
In present embodiment, luminescent layer 3 is made by following steps:
First, by Me
2si
5n
8: xSm
3+the stoichiometric ratio of each element takes Me
3n
2, Si
3n
4with SmN powder and mix sintering at 900 DEG C～1300 DEG C and within 0.5 hour～5 hours, make target, wherein x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
In this step, preferred, x is 0.03, and at 1250 DEG C, 3 hours one-tenth diameters of sintering are 50mm, the ceramic target that thickness is 2mm.
In this step, preferred, described Me
3n
2, Si
3n
4with the mol ratio of SmN powder be 2:5:(0.03～0.15).
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 0.2Pa～4Pa, the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C, sputtering power 80～300W, is then filmed, and forms luminescent layer 3 on anode 2.
In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 2Pa, and working gas is oxygen, and the flow of working gas is 25sccm, and underlayer temperature is 500 DEG C, sputtering power 100W.
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
Selecting purity is 99.99% powder, by the Zn of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.09mmol, after even mixing, at 1250 DEG C, 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.The vacuum tightness of cavity is extracted into 5.0 × 10 with mechanical pump and molecular pump
-4pa, the working gas flow of oxygen is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C, sputtering power 100W, obtaining chemical formula is Zn
2si
5n
8: 0.03Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula of the samarium doped silicon nitride light-emitting film obtaining in the present embodiment is Zn
2si
5n
8: 0.03Sm
3+, wherein Zn
2si
5n
8matrix, Sm
3+it is active element.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the samarium doped silicon nitride light-emitting film obtaining.As seen from Figure 2, in electroluminescence spectrum, there is very strong glow peak at 638nm and 727nm wavelength zone, can be applied in thin-film electroluminescent displays.
Refer to Fig. 3, Fig. 3 is the XRD curve of the samarium doped silicon nitride light-emitting film prepared of embodiment 1, test comparison standard P DF card.As can be seen from Figure 3 the diffraction peak in figure is the peak crystallization of silicon nitride, does not occur 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 graph of relation between voltage and current density and voltage and the brightness of the membrane electro luminescent device prepared of embodiment 1, 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 88cd/m
2, show that device has the good characteristics of luminescence.
Embodiment 2
Selecting purity is 99.99% powder, by the Zn of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.03mmol, after even mixing, at 900 DEG C, 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 DEG C, sputtering power 80W.Obtaining chemical formula is Zn
2si
5n
8: 0.01Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 3
Selecting purity is 99.99% powder, by the Zn of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.15mmol, after even mixing, at 1300 DEG C, 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-5pa, the working gas flow of argon gas is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, sputtering power 300W.Obtaining chemical formula is Zn
2si
5n
8: 0.05Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 4
Selecting purity is 99.99% powder, by the Mg of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.09mmol, after even mixing, at 1250 DEG C, 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.The vacuum tightness of cavity is extracted into 5.0 × 10 with mechanical pump and molecular pump
-4pa, the working gas flow of oxygen is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C, sputtering power 100W.Obtaining chemical formula is Mg
2si
5n
8: 0.03Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 5
Selecting purity is 99.99% powder, by the Mg of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.03mmol, after even mixing, at 900 DEG C, 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 DEG C, and sputtering power is 80W.Obtaining chemical formula is Mg
2si
5n
8: 0.01Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 6
Selecting purity is 99.99% powder, by the Mg of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.15mmol, after even mixing, at 1300 DEG C, 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-5pa, the working gas flow of oxygen is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, sputtering power 300W.Obtaining chemical formula is Mg
2si
5n
8: 0.05Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 7
Selecting purity is 99.99% powder, by the Ca of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.09mmol, after even mixing, at 1250 DEG C, 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.The vacuum tightness of cavity is extracted into 5.0 × 10 with mechanical pump and molecular pump
-4pa, the working gas flow of oxygen is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C, sputtering power 100W.Obtaining chemical general formula is Ca
2si
5n
8: 0.03Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 8
Selecting purity is 99.99% powder, by the Ca of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.03mmol, after even mixing, at 900 DEG C, 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 DEG C, and sputtering power is 80W.Obtaining chemical formula is Ca
2si
5n
8: 0.01Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 9
Selecting purity is 99.99% powder, by the Ca of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.15mmol, after even mixing, at 1300 DEG C, 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-5pa, the working gas flow of oxygen is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, sputtering power 300W.Obtaining chemical formula is Ca
2si
5n
8: 0.05Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 10
Selecting purity is 99.99% powder, by the Sr of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.09mmol, after even mixing, at 1250 DEG C, 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.The vacuum tightness of cavity is extracted into 5.0 × 10 with mechanical pump and molecular pump
-4pa, the working gas flow of oxygen is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C, sputtering power 100W.Obtaining chemical general formula is Sr
2si
5n
8: 0.03Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 11
Selecting purity is 99.99% powder, by the Sr of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.03mmol, after even mixing, at 900 DEG C, 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 DEG C, and sputtering power is 80W.Obtaining chemical formula is Sr
2si
5n
8: 0.01Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 12
Selecting purity is 99.99% powder, by the Sr of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.15mmol, after even mixing, at 1300 DEG C, 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-5pa, the working gas flow of oxygen is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, sputtering power 300W.Obtaining chemical formula is Sr
2si
5n
8: 0.05Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 13
Selecting purity is 99.99% powder, by the Ba of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.09mmol, after even mixing, at 1250 DEG C, 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.The vacuum tightness of cavity is extracted into 5.0 × 10 with mechanical pump and molecular pump
-4pa, the working gas flow of oxygen is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 DEG C, sputtering power 100W.Obtaining chemical general formula is Ba
2si
5n
8: 0.03Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 14
Selecting purity is 99.99% powder, by the Ba of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.03mmol, after even mixing, at 900 DEG C, 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 DEG C, and sputtering power is 80W.Obtaining chemical formula is Ba
2si
5n
8: 0.01Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 15
Selecting purity is 99.99% powder, by the Ba of 2mmol
3n
2, the Si of 5mmol
3n
4, the SmN powder of 0.15mmol, after even mixing, at 1300 DEG C, 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-5pa, the working gas flow of oxygen is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, sputtering power 300W.Obtaining chemical formula is Ba
2si
5n
8: 0.05Sm
3+light-emitting film, then evaporation one deck Ag on light-emitting film, 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. a samarium doped silicon nitride luminescent material, is characterized in that: its chemical formula is Me
2si
5n
8: xSm
3+, wherein Me
2si
5n
8be matrix, samarium ion is active element, and x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
2. a preparation method for samarium doped silicon nitride luminescent material, is characterized in that, comprises the following steps:
According to Me
2si
5n
8: xSm
3+the stoichiometric ratio of each element takes Me
3n
2, Si
3n
4with SmN powder and mix, wherein, x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element; And
The powder mixing sintering at 900 DEG C～1300 DEG C is obtained to chemical formula for 0.5 hour～5 hours is Me
2si
5n
8: xSm
3+samarium doped silicon nitride luminescent material.
3. a samarium doped silicon nitride light-emitting film, is characterized in that, the chemical general formula of the material of this samarium doped silicon nitride light-emitting film is Me
2si
5n
8: xSm
3+, wherein Me
2si
5n
8be matrix, samarium ion is active element, and x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
4. a preparation method for samarium doped silicon nitride light-emitting film, is characterized in that, comprises the following steps:
According to Me
2si
5n
8: xSm
3+the stoichiometric ratio of each element takes Me
3n
2, Si
3n
4with SmN powder and mix sintering at 900 DEG C～1300 DEG C and make target in 0.5 hour～5 hours, wherein, x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element;
Described 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; And
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C, sputtering power 80～300W, is then filmed, and obtaining chemical formula is Me
2si
5n
8: xSm
3+samarium doped silicon nitride light-emitting film.
5. the preparation method of samarium doped silicon nitride light-emitting film according to claim 4, is characterized in that, described Me
3n
2, Si
3n
4with the mol ratio of SmN powder be 2:5:(0.03～0.15).
6. the preparation method of samarium doped silicon nitride light-emitting film according to claim 4, is characterized in that, the vacuum tightness of described vacuum cavity is 5.0 × 10
-4pa, base target spacing is 60mm, and magnetron sputtering operating pressure is 2Pa, and working gas is oxygen, and the flow of working gas is 25sccm, underlayer temperature is 500 DEG C, sputtering power 100W.
7. a membrane electro luminescent device, this membrane electro luminescent device comprises the substrate, anode layer, luminescent layer and the cathode layer that stack gradually, it is characterized in that, the material of described luminescent layer is samarium doped silicon nitride luminescent material, and the chemical formula of this samarium doped silicon nitride luminescent material is Me
2si
5n
8: xSm
3+, wherein Me
2si
5n
8be matrix, samarium ion is active element, and x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
8. 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 samarium doped silicon nitride luminescent material, and the chemical formula of this samarium doped silicon nitride luminescent material is Me
2si
5n
8: xSm
3+, wherein Me
2si
5n
8be matrix, samarium ion is active element, and x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element;
On described luminescent layer, form negative electrode.
9. the preparation method of membrane electro luminescent device according to claim 8, is characterized in that, the preparation of described luminescent layer comprises the following steps:
According to Me
2si
5n
8: xSm
3+the stoichiometric ratio of each element takes Me
3n
2, Si
3n
4with SmN powder and mix sintering at 900 DEG C～1300 DEG C and within 0.5 hour～5 hours, make target, wherein x is that 0.01～0.05, Me is the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element;
Described target and described 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;
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C, sputtering power 80～300W, then be filmed, on described anode, form luminescent layer.
10. the preparation method of membrane electro luminescent device according to claim 9, is characterized in that, described Me
3n
2, Si
3n
4with the mol ratio of SmN powder be 2:5:(0.03～0.15).
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