CN104119914A - Cerium doped rare earth thiogallate luminescent material and preparation method and application thereof - Google Patents
Cerium doped rare earth thiogallate luminescent material and preparation method and application thereof Download PDFInfo
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- CN104119914A CN104119914A CN201310150006.2A CN201310150006A CN104119914A CN 104119914 A CN104119914 A CN 104119914A CN 201310150006 A CN201310150006 A CN 201310150006A CN 104119914 A CN104119914 A CN 104119914A
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Abstract
A cerium doped rare earth thiogallate luminescent material has a chemical formula of Me2GaS3:xCe<3+>, wherein x is 0.01-0.05, Me is yttrium ion, lanthanum ion, gadolinium ion or lutetium ion. In an electroluminescence (EL) spectrum of a luminescent thin film prepared from the cerium doped rare earth thiogallate luminescent material, a wavelength region of 610 nm has very strong luminescence peaks, and the luminescent thin film can be used in a thin-film electroluminescent display. The invention also provides a preparation method and application of the cerium doped rare earth thiogallate luminescent material.
Description
[technical field]
The present invention relates to the rare earth doped sulfur gallate luminescent material of a kind of cerium, its preparation method, the rare earth doped sulfur gallate light-emitting film of cerium, 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 rare earth doped sulfur gallate luminescent material of cerium 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 rare earth doped sulfur gallate luminescent material of cerium, its preparation method, the rare earth doped sulfur gallate light-emitting film of cerium, its preparation method that can be applicable to membrane electro luminescent device, use membrane electro luminescent device of the rare earth doped sulfur gallate luminescent material of this cerium and preparation method thereof.
The rare earth doped sulfur gallate luminescent material of cerium, its chemical formula is Me
2gaS
3: xCe
3+, wherein, x is that 0.01~0.05, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
A preparation method for the rare earth doped sulfur gallate luminescent material of cerium, comprises the following steps:
According to Me
2gaS
3: xCe
3+the stoichiometric ratio of each element takes Me
2s
3, Ga
2s
3and CeS
2powder also mixes, and wherein, x is 0.01~0.05; And
The powder mixing sintering at 900 ℃~1300 ℃ is obtained to chemical formula for 0.5 hour~5 hours is Me
2gaS
3: xCe
3+the rare earth doped sulfur gallate luminescent material of cerium, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
The rare earth doped sulfur gallate light-emitting film of cerium, the chemical general formula of the material of the rare earth doped sulfur gallate light-emitting film of this cerium is Me
2gaS
3: xCe
3+, wherein, x is that 0.01~0.05, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
A preparation method for the rare earth doped sulfur gallate light-emitting film of cerium, comprises the following steps:
According to Me
2gaS
3: xCe
3+the stoichiometric ratio of each element takes Me
2s
3, Ga
2s
3and CeS
2powder also mixes sintering at 900 ℃~1300 ℃ and makes target in 0.5 hour~5 hours, and wherein, x is 0.01~0.05;
The vacuum cavity that described target and substrate is packed into magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3pa~1.0 * 10
-5pa; And
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm~95mm, magnetron sputtering operating pressure 0.5Pa~5Pa, and the flow of working gas is 10sccm~40sccm, underlayer temperature is 250 ℃~750 ℃, laser energy is 80W~300W, is then filmed, and obtaining chemical formula is Me
2gaS
3: xCe
3+the rare earth doped sulfur gallate light-emitting film of cerium, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
In a preferred embodiment, the vacuum tightness of described vacuum cavity is 5.0 * 10
-4pa, base target spacing is 60mm, and magnetron sputtering operating pressure is 3Pa, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃, and laser energy is 150W.
A kind of membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer stacking gradually, the material of described luminescent layer is the rare earth doped sulfur gallate luminescent material of cerium, and the chemical formula of the rare earth doped sulfur gallate luminescent material of this cerium is Me
2gaS
3: xCe
3+, wherein, x is that 0.01~0.05, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
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 the rare earth doped sulfur gallate luminescent material of cerium, and the chemical formula of the rare earth doped sulfur gallate luminescent material of this cerium is Me
2gaS
3: xCe
3+, wherein, x is that 0.01~0.05, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion;
On described luminescent layer, form negative electrode.
In a preferred embodiment, the preparation of described luminescent layer comprises the following steps:
According to Me
2gaS
3: xCe
3+the stoichiometric ratio of each element takes Me
2s
3, Ga
2s
3and CeS
2powder also mixes sintering at 900 ℃~1300 ℃ and makes target in 0.5 hour~5 hours, and wherein, x is 0.01~0.05;
The vacuum cavity that described target and described substrate is packed into magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3pa~1.0 * 10
-5pa;
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm~95mm, magnetron sputtering operating pressure 0.5Pa~5Pa, and the flow of working gas is 10sccm~340sccm, underlayer temperature is 250 ℃~750 ℃, laser energy is 80W~300W, is then filmed, and obtaining chemical formula is Me
2gaS
3: xCe
3+the rare earth doped sulfur gallate light-emitting film of cerium, on described anode, form luminescent layer.
The rare earth doped sulfur gallate luminescent material of above-mentioned cerium (Me
2gaS
3: xCe
3+) in the electroluminescent spectrum (EL) of the light-emitting film made, in 610nm wavelength zone, there is very strong glow peak, can be applied in thin-film electroluminescent displays.
[accompanying drawing explanation]
Fig. 1 is the structural representation of the membrane electro luminescent device of an embodiment;
Fig. 2 is the electroluminescent spectrogram of the rare earth doped sulfur gallate light-emitting film of cerium of embodiment 1 preparation;
Fig. 3 is the XRD figure of the rare earth doped sulfur gallate light-emitting film of cerium of embodiment 1 preparation;
Fig. 4 is the voltage of membrane electro luminescent device of embodiment 1 preparation and the graph of relation between current density and voltage and brightness.
[embodiment]
Below in conjunction with the drawings and specific embodiments, the rare earth doped sulfur gallate luminescent material of cerium, its preparation method, the rare earth doped sulfur gallate light-emitting film of cerium, its preparation method, membrane electro luminescent device and preparation method thereof are further illustrated.
The rare earth doped sulfur gallate luminescent material of cerium of one embodiment, its chemical formula is Me
2gaS
3: xCe
3+, wherein, x is that 0.01~0.05, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
Preferably, x is 0.03.
Me in the rare earth doped sulfur gallate luminescent material of this cerium
2gaS
3be matrix, cerium ion is active element.In the electroluminescent spectrum (EL) of the light-emitting film that the rare earth doped sulfur gallate luminescent material of this cerium is made, in 610nm wavelength zone, there is very strong glow peak, can be applied in thin-film electroluminescent displays.
The preparation method of the rare earth doped sulfur gallate luminescent material of above-mentioned cerium, comprises the following steps:
Step S11, according to Me
2gaS
3: xCe
3+the stoichiometric ratio of each element takes Me
2s
3, Ga
2s
3and CeS
2powder, wherein, x is 0.01~0.05.
In this step, preferred, x is 0.03.
Step S12, by mixing equal powder sintering at 900 ℃~1300 ℃, within 0.5 hour~5 hours, can obtain the rare earth doped sulfur gallate luminescent material of cerium, its chemical formula is Me
2gaS
3: xCe
3+, x is 0.01~0.05.
In this step, preferred sintering 3 hours at 1250 ℃.
The rare earth doped sulfur gallate light-emitting film of cerium of one embodiment, the chemical general formula of the material of the rare earth doped sulfur gallate light-emitting film of this cerium is Me
2gaS
3: xCe
3+the rare earth doped sulfur gallate luminescent material of cerium, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
Preferably, x is 0.03.
The preparation method of the rare earth doped sulfur gallate light-emitting film of above-mentioned cerium, comprises the following steps:
Step S21, press Me
2gaS
3: xCe
3+the stoichiometric ratio of each element takes Me
2s
3, Ga
2s
3and CeS
2powder also mixes sintering at 900 ℃~1300 ℃ and makes target in 0.5 hour~5 hours, and wherein, x is 0.01~0.05.
In this step, preferred, x is 0.03, and at 1250 ℃, 3 hours one-tenth diameters of sintering are 50mm, the ceramic target that thickness is 2mm.
Step S22, the target obtaining in step S21 and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3pa~1.0 * 10
-5pa.
In this step, preferred, vacuum tightness is 5 * 10
-4pa.
Step S23, adjustment magnetron sputtering plating processing parameter are: base target spacing is 45mm~95mm, magnetron sputtering operating pressure 0.5Pa~5Pa, and the flow of working gas is 10sccm~40sccm, underlayer temperature is 250 ℃~750 ℃; Laser energy is 80W~300W, is then filmed, and obtaining chemical formula is Me
2gaS
3: xCe
3+the rare earth doped sulfur gallate light-emitting film of cerium, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 3Pa, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃, and laser energy is 150W.
Refer to Fig. 1, the membrane electro luminescent device 100 of an embodiment, this membrane electro luminescent device 100 comprises substrate 1, anode 2, luminescent layer 3 and the negative electrode 4 stacking gradually.
Substrate 1 is glass substrate.Anode 2 is for being formed at the tin indium oxide (ITO) in glass substrate.The material of luminescent layer 3 is the rare earth doped sulfur gallate luminescent material of cerium, and the chemical formula of the rare earth doped sulfur gallate luminescent material of this cerium is Me
2gaS
3: xCe
3+, wherein, x is that 0.01~0.05, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.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 the rare earth doped sulfur gallate luminescent material of cerium, and the chemical formula of the rare earth doped sulfur gallate luminescent material of this cerium is Me
2gaS
3: xCe
3+, wherein, x is that 0.01~0.05, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
In present embodiment, luminescent layer 3 is made by following steps:
First, by Me
2gaS
3: xCe
3+the stoichiometric ratio of each element takes Me
2s
3, Ga
2s
3and CeS
2powder also mixes sintering at 900 ℃~1300 ℃ and within 0.5 hour~5 hours, makes target, and wherein x is 0.01~0.05.
In this step, preferred, x is 0.03, and at 1250 ℃, 3 hours one-tenth diameters of sintering are 50mm, the ceramic target that thickness is 2mm.
Secondly, target and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3pa~1.0 * 10
-5pa.
In this step, preferred, vacuum tightness is 5 * 10
-4pa.
Then, adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm~95mm, magnetron sputtering operating pressure 0.5Pa~5Pa, the flow of working gas is 10sccm~40sccm, underlayer temperature is 250 ℃~750 ℃, laser energy is 80W~300W, is then filmed, and forms luminescent layer 3 on anode 2.
In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 3Pa, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃, and laser energy is 150W.
Step S33, on luminescent layer 3, form negative electrode 4.
In present embodiment, the material of negative electrode 4 is silver (Ag), by evaporation, is formed.
Be specific embodiment below.
Embodiment 1
Selecting purity is 99.99% powder, by the Y of 2mmol
2s
3, the Ga of 1mmol
2s
3and 0.03mmolCeS
2powder, after even mixing, at 1250 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 60mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 5.0 * 10
-4pa, the working gas flow of oxygen is 20sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 500 ℃, laser energy 150W.The sample chemical formula obtaining is Y
2gaS
3: 0.03Ce
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
The chemical general formula of the rare earth doped sulfur gallate light-emitting film of cerium obtaining in the present embodiment is Y
2gaS
3: 0.03Ce
3+, Y wherein
2gaS
3matrix, Ce
3+it is active element.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the rare earth doped sulfur gallate light-emitting film of the cerium obtaining.As seen from Figure 2, in electroluminescence spectrum, in 610nm wavelength zone, there is very strong glow peak, can be applied in thin-film electroluminescent displays.
Refer to Fig. 3, Fig. 3 is the XRD curve of the rare earth doped sulfur gallate light-emitting film of cerium of embodiment 1 preparation, test comparison standard P DF card.As can be seen from Figure 3 diffraction peak is depicted as the peak crystallization of sulfur gallate, does not occur the diffraction peak of doped element and other impurity, illustrates that the product that this preparation method obtains has good crystalline quality.
Refer to Fig. 4, Fig. 4 is the voltage of membrane electro luminescent device of embodiment 1 preparation and the graph of relation between current density and voltage and brightness, curve 1 is voltage and current density relation curve, can find out that this device starts luminous from voltage 5.5V, curve 2 is voltage and brightness relationship curve, and the high-high brightness that can find out this device is 83cd/m
2, show that device has the good characteristics of luminescence.
Embodiment 2
Selecting purity is 99.99% powder, by the Y of 2mmol
2s
3, the Ga of 1mmol
2s
3and 0.01mmolCeS
2powder, after even mixing, at 900 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 ℃, laser energy 80W.The chemical formula of the sample obtaining is Y
2gaS
3: 0.01Ce
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 3
Selecting purity is 99.99% powder, by the Y of 2mmol
2s
3, the Ga of 1mmol
2s
3and 0.05mmolCeS
2powder, after even mixing, at 1300 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 95mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-5pa, the working gas flow of oxygen is 40sccm, and pressure is adjusted to 5.0Pa, and underlayer temperature is 750 ℃, laser energy 300W.The chemical formula of the sample obtaining is Y
2gaS
3: 0.05Ce
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 4
Selecting purity is 99.99% powder, by the La of 2mmol
2s
3, the Ga of 1mmol
2s
3and 0.03mmolCeS
2powder, after even mixing, at 1250 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 60mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 5.0 * 10
-4pa, the working gas flow of oxygen is 20sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 500 ℃, laser energy 150W.The chemical formula of the sample obtaining is La
2gaS
3: 0.03Ce
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 5
Selecting purity is 99.99% powder, by the La of 2mmol
2s
3, the Ga of 1mmol
2s
3and 0.01mmolCeS
2powder, after even mixing, at 900 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 ℃, laser energy 80W.The chemical formula of the sample obtaining is La
2gaS
3: 0.01Ce
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 6
Selecting purity is 99.99% powder, by the Y of 2mmol
2s
3, the Ga of 1mmol
2s
3and 0.05mmolCeS
2powder, after even mixing, at 1300 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 95mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-5pa, the working gas flow of oxygen is 40sccm, and pressure is adjusted to 5.0Pa, and underlayer temperature is 750 ℃, laser energy 300W.The chemical formula of the sample obtaining is La
2gaS
3: 0.05Ce
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 7
Selecting purity is 99.99% powder, by the Gd of 2mmol
2s
3, the Ga of 1mmol
2s
3and 0.03mmolCeS
2, after even mixing, at 1250 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 60mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 5.0 * 10
-4pa, the working gas flow of oxygen is 20sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 500 ℃, laser energy 150W.The chemical general formula of the sample obtaining is Gd
2gaS
3: 0.03Ce
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 8
Selecting purity is 99.99% powder, by the Gd of 2mmol
2s
3, the Ga of 1mmol
2s
3and 0.01mmolCeS
2powder, after even mixing, at 900 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 ℃, laser energy 80W.The chemical formula of the sample obtaining is Gd
2gaS
3: 0.01Ce
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 9
Selecting purity is 99.99% powder, by the Gd of 2mmol
2s
3, the Ga of 1mmol
2s
3and 0.05mmolCeS
2powder, after even mixing, at 1300 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 95mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-5pa, the working gas flow of oxygen is 40sccm, and pressure is adjusted to 5.0Pa, and underlayer temperature is 750 ℃, laser energy 300W.The chemical formula of the sample obtaining is Gd
2gaS
3: 0.05Ce
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 10
Selecting purity is 99.99% powder, by the Lu of 2mmol
2s
3, the Ga of 1mmol
2s
3and 0.03mmolCeS
2, after even mixing, at 1250 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 60mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 5.0 * 10
-4pa, the working gas flow of oxygen is 20sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 500 ℃, laser energy 150W.The chemical formula of the sample obtaining is Lu
2gaS
3: 0.03Ce
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 11
Selecting purity is 99.99% powder, by the Lu of 2mmol
2s
3, the Ga of 1mmol
2s
3and 0.01mmolCeS
2powder, after even mixing, at 900 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 ℃, laser energy 80W.The chemical formula of the sample obtaining is Lu
2gaS
3: 0.01Ce
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 12
Selecting purity is 99.99% powder, by the Lu of 2mmol
2s
3, the Ga of 1mmol
2s
3and 0.05mmolCeS
2powder, after even mixing, at 1300 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 95mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-5pa, the working gas flow of oxygen is 40sccm, and pressure is adjusted to 5.0Pa, and underlayer temperature is 750 ℃, laser energy 300W.The chemical formula of the sample obtaining is Lu
2gaS
3: 0.05Ce
3+light-emitting film, evaporation one deck Ag on light-emitting film then, as negative electrode.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. the rare earth doped sulfur gallate luminescent material of cerium, is characterized in that: its chemical formula is Me
2gaS
3: xCe
3+, wherein, x is that 0.01~0.05, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
2. a preparation method for the rare earth doped sulfur gallate luminescent material of cerium, is characterized in that, comprises the following steps:
According to Me
2gaS
3: xCe
3+the stoichiometric ratio of each element takes Me
2s
3, Ga
2s
3and CeS
2powder also mixes, and wherein, x is 0.01~0.05; And
The powder mixing sintering at 900 ℃~1300 ℃ is obtained to chemical formula for 0.5 hour~5 hours is Me
2gaS
3: xCe
3+the rare earth doped sulfur gallate luminescent material of cerium, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
3. the rare earth doped sulfur gallate light-emitting film of cerium, is characterized in that, the chemical general formula of the material of the rare earth doped sulfur gallate light-emitting film of this cerium is Me
2gaS
3: xCe
3+, wherein, x is that 0.01~0.05, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
4. a preparation method for the rare earth doped sulfur gallate light-emitting film of cerium, is characterized in that, comprises the following steps:
According to Me
2gaS
3: xCe
3+the stoichiometric ratio of each element takes Me
2s
3, Ga
2s
3and CeS
2powder also mixes sintering at 900 ℃~1300 ℃ and makes target in 0.5 hour~5 hours, and wherein, x is 0.01~0.05;
The vacuum cavity that described target and substrate is packed into magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3pa~1.0 * 10
-5pa; And
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm~95mm, magnetron sputtering operating pressure 0.5Pa~5Pa, and the flow of working gas is 10sccm~40sccm, underlayer temperature is 250 ℃~750 ℃, laser energy is 80W~300W, is then filmed, and obtaining chemical formula is Me
2gaS
3: xCe
3+the rare earth doped sulfur gallate light-emitting film of cerium, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
5. the preparation method of the rare earth doped sulfur gallate light-emitting film of cerium according to claim 4, is characterized in that, the vacuum tightness of described vacuum cavity is 5.0 * 10
-4pa, base target spacing is 60mm, and magnetron sputtering operating pressure is 3Pa, and working gas is oxygen, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃, and laser energy is 150W.
6. a membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer stacking gradually, it is characterized in that, the material of described luminescent layer is the rare earth doped sulfur gallate luminescent material of cerium, and the chemical formula of the rare earth doped sulfur gallate luminescent material of this cerium is Me
2gaS
3: xCe
3+, wherein, x is that 0.01~0.05, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion.
7. a preparation method for membrane electro luminescent device, is characterized in that, comprises the following steps:
The substrate with anode is provided;
On described anode, form luminescent layer, the material of described luminescent layer is the rare earth doped sulfur gallate luminescent material of cerium, and the chemical formula of the rare earth doped sulfur gallate luminescent material of this cerium is Me
2gaS
3: xCe
3+, wherein, x is that 0.01~0.05, Me is ruthenium ion, lanthanum ion, gadolinium ion or lutetium ion;
On described luminescent layer, form negative electrode.
8. the preparation method of membrane electro luminescent device according to claim 7, is characterized in that, the preparation of described luminescent layer comprises the following steps:
According to Me
2gaS
3: xCe
3+the stoichiometric ratio of each element takes Me
2s
3, Ga
2s
3and CeS
2powder also mixes sintering at 900 ℃~1300 ℃ and makes target in 0.5 hour~5 hours, and wherein, x is 0.01~0.05;
The vacuum cavity that described target and described substrate is packed into magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3pa~1.0 * 10
-5pa;
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm~95mm, magnetron sputtering operating pressure 0.5Pa~5Pa, and the flow of working gas is 10sccm~40sccm, underlayer temperature is 250 ℃~750 ℃, laser energy is 80W~300W, is then filmed, and obtaining chemical formula is Me
2gaS
3: xCe
3+the rare earth doped sulfur gallate light-emitting film of cerium, on described anode, form luminescent layer.
9. the preparation method of membrane electro luminescent device according to claim 8, is characterized in that, described x is 0.03.
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CN102838985A (en) * | 2011-06-22 | 2012-12-26 | 海洋王照明科技股份有限公司 | Titanium-doped strontium thio-aluminate luminescent film, preparation method thereof, and organic electroluminescent device |
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