CN104140813A - Manganese-chromium-codoped silicon-aluminium oxynitride alkaline-earth salt luminescent material, preparation method and application thereof - Google Patents

Manganese-chromium-codoped silicon-aluminium oxynitride alkaline-earth salt luminescent material, preparation method and application thereof Download PDF

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CN104140813A
CN104140813A CN201310168141.XA CN201310168141A CN104140813A CN 104140813 A CN104140813 A CN 104140813A CN 201310168141 A CN201310168141 A CN 201310168141A CN 104140813 A CN104140813 A CN 104140813A
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earth salt
sialon
alkaline earth
altogether
nitrogen oxygen
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周明杰
王平
陈吉星
钟铁涛
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

A manganese-chromium-codoped silicon-aluminium oxynitride alkaline-earth salt luminescent material is disclosed. The chemical formula of the luminescent material is Me-SiAlON:xMn4<+>, yCr4<+>, wherein Me-SiAlON is a matrix; Mn4<+> ion and Cr4<+> ion are active elements; x is 0.01-0.07; y is 0.01-0.05; and Me is one element selected from zinc element, magnesium element, calcium element, strontium element and barium element. In the electroluminescence spectra (EL) of a luminescent thin-film prepared from the manganese-chromium-codoped silicon-aluminium oxynitride alkaline-earth salt luminescent material, there is strong luminescence peak at wavelengths of 607nm and 629nm, and the luminescent thin-film can be applied in a thin-film electroluminescent display. The invention also provides a preparation method of the manganese-chromium-codoped silicon-aluminium oxynitride alkaline-earth salt luminescent material and its application.

Description

Manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material, preparation method and application thereof altogether
[technical field]
The present invention relates to a kind of manganese chromium mixes altogether sial nitrogen oxygen alkaline earth salt luminescent material, its preparation method, manganese chromium and mixes altogether sial nitrogen oxygen alkaline earth salt 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 the manganese chromium that can be applicable to thin-film electroluminescent displays is mixed sial nitrogen oxygen alkaline earth salt luminescent material altogether, has not yet to see report.
[summary of the invention]
Based on this, be necessary to provide a kind of manganese chromium that can be applicable to membrane electro luminescent device to mix altogether sial nitrogen oxygen alkaline earth salt luminescent material, its preparation method, manganese chromium and mix altogether sial nitrogen oxygen alkaline earth salt light-emitting film, its preparation method, use this manganese chromium to mix altogether membrane electro luminescent device of sial nitrogen oxygen alkaline earth salt luminescent material and preparation method thereof.
A kind of manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material altogether, and its chemical formula is Me-SiAlON:xMn 4+, yCr 4+, Me-SiAlON is matrix, Mn 4+ion and Cr 4+ion is active element, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
Described x is that 0.04, y is 0.02.
Manganese chromium is mixed a preparation method for sial nitrogen oxygen alkaline earth salt luminescent material altogether, comprises the following steps:
According to Me-SiAlON:xMn 4+, yCr 4+the stoichiometric ratio of each element takes MeO, Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder also mixes, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from 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-SiAlON:xMn 4+, yCr 4+manganese chromium mix altogether sial nitrogen oxygen alkaline earth salt luminescent material.
A kind of manganese chromium is mixed sial nitrogen oxygen alkaline earth salt light-emitting film altogether, and the chemical general formula that this manganese chromium is mixed the material of sial nitrogen oxygen alkaline earth salt light-emitting film is altogether Me-SiAlON:xMn 4+, yCr 4+, Me-SiAlON is matrix, Mn 4+ion and Cr 4+ion is active element, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
Manganese chromium is mixed a preparation method for sial nitrogen oxygen alkaline earth salt light-emitting film altogether, comprises the following steps:
According to Me-SiAlON:xMn 4+, yCr 4+the stoichiometric ratio of each element takes MeO, Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder also mixes, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from 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, the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C, then be filmed, obtaining chemical formula is Me-SiAlON:xMn 4+, yCr 4+manganese chromium mix altogether sial nitrogen oxygen alkaline earth salt light-emitting film.
Also comprise step: described manganese chromium is mixed to the vacuum annealing at 500 DEG C～800 DEG C of sial nitrogen oxygen alkaline earth salt light-emitting film altogether and process 1h～3h.
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, the material of described luminescent layer is that manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material altogether, and the chemical formula that this manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material is altogether Me-SiAlON:xMn 4+, yCr 4+, Me-SiAlON is matrix, Mn 4+ion and Cr 4+ion is active element, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from 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 that manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material altogether, and the chemical formula that this manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material is altogether Me-SiAlON:xMn 4+, yCr 4+, Me-SiAlON is matrix, Mn 4+ion and Cr 4+ion is active element, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element;
On described luminescent layer, form negative electrode.
The preparation of described luminescent layer comprises the following steps:
According to Me-SiAlON:xMn 4+, yCr 4+the stoichiometric ratio of each element takes MeO, Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder also mixes, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from 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, then be filmed, on described anode, form luminescent layer.
Also comprise step: described manganese chromium is mixed to the vacuum annealing at 500 DEG C～800 DEG C of sial nitrogen oxygen alkaline earth salt light-emitting film altogether and process 1h～3h.
Above-mentioned manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material (Me-SiAlON:xMn altogether 4+, yCr 4+) in the electroluminescent spectrum (EL) of the light-emitting film made, there is very strong glow peak at 607nm and 629nm 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 that manganese chromium prepared by embodiment 1 is mixed sial nitrogen oxygen alkaline earth salt light-emitting film altogether;
Fig. 3 is the Raman spectrum that manganese chromium prepared by embodiment 1 is mixed sial nitrogen oxygen alkaline earth salt light-emitting film altogether;
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, manganese chromium being mixed to sial nitrogen oxygen alkaline earth salt luminescent material, its preparation method, manganese chromium altogether mixes altogether sial nitrogen oxygen alkaline earth salt light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof and further illustrates.
The manganese chromium of one embodiment is mixed sial nitrogen oxygen alkaline earth salt luminescent material altogether, and its chemical formula is Me-SiAlON:xMn 4+, yCr 4+, Me-SiAlON is matrix, Mn 4+ion and Cr 4+ion is active element, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
Preferably, x is that 0.04, y is 0.02.
This manganese chromium is mixed in the electroluminescent spectrum (EL) of the light-emitting film that sial nitrogen oxygen alkaline earth salt luminescent material makes altogether, has very strong glow peak at 607nm and 629nm wavelength zone, can be applied in thin-film electroluminescent displays.
Above-mentioned manganese chromium is mixed the preparation method of sial nitrogen oxygen alkaline earth salt luminescent material altogether, comprises the following steps:
Step S11, according to Me-SiAlON:xMn 4+, yCr 4+the stoichiometric ratio of each element takes MeO, Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder also mixes, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from 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-SiAlON:xMn 4+, yCr 4+manganese chromium mix altogether sial nitrogen oxygen alkaline earth salt luminescent material.
In this step, preferred, x is that 0.04, y is 0.02.
In this step, preferred, MeO, Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3the molar mass of powder is than being (5～20): (60～75): (3～10): (0.5～5): (0.5～10);
More preferably, MeO, Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3the molar mass of powder is than being 15:68:8:3:6.
Step S12, within 0.5 hour～5 hours, can obtain manganese chromium and mix altogether sial nitrogen oxygen alkaline earth salt luminescent material mixing equal powder sintering at 900 DEG C～1300 DEG C, its chemical formula is Me-SiAlON:xMn 4+, yCr 4+.
In this step, preferably sintering 3 hours at 1250 DEG C.
The manganese chromium of one embodiment is mixed sial nitrogen oxygen alkaline earth salt light-emitting film altogether, and the chemical general formula that this manganese chromium is mixed the material of sial nitrogen oxygen alkaline earth salt light-emitting film is altogether Me-SiAlON:xMn 4+, yCr 4+, Me-SiAlON is matrix, Mn 4+ion and Cr 4+ion is active element, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
Preferably, x is that 0.04, y is 0.02.
Above-mentioned manganese chromium is mixed the preparation method of sial nitrogen oxygen alkaline earth salt light-emitting film altogether, comprises the following steps:
Step S21, press Me-SiAlON:xMn 4+, yCr 4+the stoichiometric ratio of each element takes MeO, Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder also mixes, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
In this step, preferred, x is that 0.04, y is 0.02, 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, MeO, Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3the molar mass of powder is than being (5～20): (60～75): (3～10): (0.5～5): (0.5～10);
More preferably, MeO, Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3the molar mass of powder is than being 15:68:8:3:6.
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, and the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C; Then be filmed, obtaining chemical formula is Me-SiAlON:xMn 4+, yCr 4+manganese chromium mix altogether sial nitrogen oxygen alkaline earth salt light-emitting film.
Also comprise step: described manganese chromium is mixed to the vacuum annealing at 500 DEG C～800 DEG C of sial nitrogen oxygen alkaline earth salt light-emitting film altogether and process 1h～3h.
In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 2Pa, and working gas is oxygen, and the flow of working gas is 25sccm, and underlayer temperature is 500 DEG C.
Refer to Fig. 1, the membrane electro luminescent device 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 that manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material altogether, and the chemical formula that this manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material is altogether Me-SiAlON:xMn 4+, yCr 4+, Me-SiAlON is matrix, Mn 4+ion and Cr 4+ion is active element, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from 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 that manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material altogether, and the chemical formula that this manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material is altogether Me-SiAlON:xMn 4+, yCr 4+, Me-SiAlON is matrix, Mn 4+ion and Cr 4+ion is active element, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from 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-SiAlON:xMn 4+, yCr 4+the stoichiometric ratio of each element takes MeO, Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder also mixes, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
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, 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, and laser energy is 300W.
Also comprise step: described manganese chromium is mixed to the vacuum annealing at 500 DEG C～800 DEG C of sial nitrogen oxygen alkaline earth salt light-emitting film altogether and process 1h～3h.
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 ZnO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass ratio for 15:68:8:3 is after even mixing, and 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.The sample chemical formula obtaining is Zn-SiAlON:0.03Mn 4+, 0.06Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 600 DEG C, anneal 2h, then evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula that the manganese chromium obtaining in the present embodiment is mixed sial nitrogen oxygen alkaline earth salt light-emitting film is altogether Zn-SiAlON:0.03Mn 4+, 0.06Cr 4+.
Refer to Fig. 2, Figure 2 shows that the manganese chromium obtaining mixes the electroluminescence spectrum (EL) of sial nitrogen oxygen alkaline earth salt light-emitting film altogether.As seen from Figure 2, in electroluminescence spectrum, there is very strong glow peak at 607nm and 629nm wavelength zone, can be applied in thin-film electroluminescent displays.
Refer to Fig. 3, Fig. 3 is the Raman spectrum that manganese chromium prepared by embodiment 1 is mixed sial nitrogen oxygen alkaline earth salt light-emitting film altogether, Raman peaks is depicted as sial nitrogen oxygen alkaline earth salt glass characteristic peak as seen from the figure, there is not the peak of doped element and other impurity, illustrate that doped element and substrate material have formed good bonding.
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 5.5V, curve 2 is voltage and brightness relationship curve, and the high-high brightness that can find out this device is 89cd/m 2, show that device has the good characteristics of luminescence.
Embodiment 2
Selecting purity is 99.99% powder, by ZnO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass than being 20:75:4:0.5:0.05, and 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 0.2Pa, and underlayer temperature is 250 DEG C, and the chemical formula of the sample obtaining is Zn-SiAlON:0.005Mn 4+, 0.005Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 500 DEG C, anneal 1h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 3
Selecting purity is 99.99% powder, by ZnO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass than being 5:70:10:5:10, and 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, and the chemical formula of the sample obtaining is Zn-SiAlON:0.05Mn 4+, 0.1Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 800 DEG C, anneal 3h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 4
Selecting purity is 99.99% powder, by MgO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass ratio for 15:68:8:3 is after even mixing, and 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.The sample chemical formula obtaining is Mg-SiAlON:0.03Mn 4+, 0.06Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 600 DEG C, anneal 2h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 5
Selecting purity is 99.99% powder, by MgO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass than being 20:75:4:0.5:0.05, and 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 0.2Pa, and underlayer temperature is 250 DEG C, and the chemical formula of the sample obtaining is Mg-SiAlON:0.005Mn 4+, 0.005Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 500 DEG C, anneal 1h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 6
Selecting purity is 99.99% powder, by MgO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass than being 5:70:10:5:10, and 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, and the chemical formula of the sample obtaining is Mg-SiAlON:0.05Mn 4+, 0.1Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 800 DEG C, anneal 3h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 7
Selecting purity is 99.99% powder, by CaO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass ratio for 15:68:8:3 is after even mixing, and 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.The sample chemical formula obtaining is Zn-SiAlON:0.03Mn 4+, 0.06Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 600 DEG C, anneal 2h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 8
Selecting purity is 99.99% powder, by CaO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass than being 20:75:4:0.5:0.05, and 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 0.2Pa, and underlayer temperature is 250 DEG C, and the chemical formula of the sample obtaining is Ca-SiAlON:0.005Mn 4+, 0.005Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 500 DEG C, anneal 1h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 9
Selecting purity is 99.99% powder, by CaO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass than being 5:70:10:5:10, and 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, and the chemical formula of the sample obtaining is Ca-SiAlON:0.05Mn 4+, 0.1Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 800 DEG C, anneal 3h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 10
Selecting purity is 99.99% powder, by SrO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass ratio for 15:68:8:3 is after even mixing, and 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.The sample chemical formula obtaining is Sr-SiAlON:0.03Mn 4+, 0.06Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 600 DEG C, anneal 2h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 11
Selecting purity is 99.99% powder, by SrO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass than being 20:75:4:0.5:0.05, and 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 0.2Pa, and underlayer temperature is 250 DEG C, and the chemical formula of the sample obtaining is Sr-SiAlON:0.005Mn 4+, 0.005Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 500 DEG C, anneal 1h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 12
Selecting purity is 99.99% powder, by SrO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass than being 5:70:10:5:10, and 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, and the chemical formula of the sample obtaining is Sr-SiAlON:0.05Mn 4+, 0.1Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 800 DEG C, anneal 3h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 13
Selecting purity is 99.99% powder, by BaO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass ratio for 15:68:8:3 is after even mixing, and 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.The sample chemical formula obtaining is Ba-SiAlON:0.03Mn 4+, 0.06Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 600 DEG C, anneal 2h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 14
Selecting purity is 99.99% powder, by BaO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass than being 20:75:4:0.5:0.05, and 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 0.2Pa, and underlayer temperature is 250 DEG C, and the chemical formula of the sample obtaining is Ba-SiAlON:0.005Mn 4+, 0.005Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 500 DEG C, anneal 1h, then evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 15
Selecting purity is 99.99% powder, by BaO, and Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder is according to molar mass than being 5:70:10:5:10, and 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, and the chemical formula of the sample obtaining is Ba-SiAlON:0.05Mn 4+, 0.1Cr 4+light-emitting film, be then 0.01Pa by the light-emitting film obtaining vacuum tightness in vacuum tightness, annealing temperature is 800 DEG C, anneal 3h, then evaporation one deck Ag on light-emitting film, as negative electrode.
The above embodiment 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. manganese chromium is mixed a sial nitrogen oxygen alkaline earth salt luminescent material altogether, it is characterized in that: its chemical formula is Me-SiAlON:xMn 4+, yCr 4+, Me-SiAlON is matrix, Mn 4+ion and Cr 4+ion is active element, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
2. luminescent material according to claim 1, is characterized in that: described x is that 0.04, y is 0.02.
3. manganese chromium is mixed a preparation method for sial nitrogen oxygen alkaline earth salt luminescent material altogether, it is characterized in that, comprises the following steps:
According to Me-SiAlON:xMn 4+, yCr 4+the stoichiometric ratio of each element takes MeO, Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder also mixes, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from 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-SiAlON:xMn 4+, yCr 4+manganese chromium mix altogether sial nitrogen oxygen alkaline earth salt luminescent material.
4. manganese chromium is mixed a sial nitrogen oxygen alkaline earth salt light-emitting film altogether, it is characterized in that, the chemical general formula that this manganese chromium is mixed the material of sial nitrogen oxygen alkaline earth salt light-emitting film is altogether Me-SiAlON:xMn 4+, yCr 4+, Me-SiAlON is matrix, Mn 4+ion and Cr 4+ion is active element, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from the one in zinc element, magnesium elements, calcium constituent, strontium element and barium element.
5. manganese chromium is mixed a preparation method for sial nitrogen oxygen alkaline earth salt light-emitting film altogether, it is characterized in that, comprises the following steps:
According to Me-SiAlON:xMn 4+, yCr 4+the stoichiometric ratio of each element takes MeO, Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder also mixes, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from 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, the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 DEG C～750 DEG C, then be filmed, obtaining chemical formula is Me-SiAlON:xMn 4+, yCr 4+manganese chromium mix altogether sial nitrogen oxygen alkaline earth salt light-emitting film.
6. manganese chromium according to claim 5 is mixed the preparation method of sial nitrogen oxygen alkaline earth salt light-emitting film altogether, it is characterized in that, also comprises step: described manganese chromium is mixed to the vacuum annealing at 500 DEG C～800 DEG C of sial nitrogen oxygen alkaline earth salt light-emitting film altogether and process 1h～3h.
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 that manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material altogether, and the chemical formula that this manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material is altogether Me-SiAlON:xMn 4+, yCr 4+, Me-SiAlON is matrix, Mn 4+ion and Cr 4+ion is active element, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from 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 that manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material altogether, and the chemical formula that this manganese chromium is mixed sial nitrogen oxygen alkaline earth salt luminescent material is altogether Me-SiAlON:xMn 4+, yCr 4+, Me-SiAlON is matrix, Mn 4+ion and Cr 4+ion is active element, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from 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-SiAlON:xMn 4+, yCr 4+the stoichiometric ratio of each element takes MeO, Si 3n 4, Al 2o 3, MnO 2and Cr 2o 3powder also mixes, and wherein, x is that 0.01～0.07, y is that 0.01～0.05, Me is selected from 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, then be filmed, on described anode, form luminescent layer.
10. the preparation method of membrane electro luminescent device according to claim 8, is characterized in that, also comprises step: described manganese chromium is mixed to the vacuum annealing at 500 DEG C～800 DEG C of sial nitrogen oxygen alkaline earth salt light-emitting film altogether and process 1h～3h.
CN201310168141.XA 2013-05-06 2013-05-06 Manganese-chromium-codoped silicon-aluminium oxynitride alkaline-earth salt luminescent material, preparation method and application thereof Pending CN104140813A (en)

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Application publication date: 20141112