CN104178137A - Praseodymium-doped indium silicate luminescent film, preparing method thereof and electroluminescent device - Google Patents
Praseodymium-doped indium silicate luminescent film, preparing method thereof and electroluminescent device Download PDFInfo
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- CN104178137A CN104178137A CN201310195304.3A CN201310195304A CN104178137A CN 104178137 A CN104178137 A CN 104178137A CN 201310195304 A CN201310195304 A CN 201310195304A CN 104178137 A CN104178137 A CN 104178137A
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Abstract
The invention belongs to the field of photoelectric materials, and discloses praseodymium-doped indium silicate luminescent film, a preparing method thereof and an electroluminescent device. The general chemical formula of the luminescent film is MeIn<2-x>Si2O8:xPr<3+>, wherein the MeIn<2-x>Si2O8 is a substrate, the Pr<3+> is an activating optical ion and is the luminescent center of the luminescent film, the Me is selected from Mg, Ca, Sr or Ba, and the x is 0.01-0.05. In an electroluminescence (EL) spectrum of the luminescent film, a strong luminescence peak is formed at 625 nm.
Description
Technical field
The present invention relates to field of photovoltaic materials, relate in particular to light-emitting film of a kind of praseodymium doped indium silicate and preparation method thereof.The invention still further relates to a kind of this light-emitting film that uses as the electroluminescent device of luminescent layer.
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.
In the research of LED fluorescent material, rear-earth-doped indium silicate fluorescent powder, its excitation spectrum can mate existing near ultraviolet preferably, and the emmission spectrum of LED can access good green glow exciting to blue light.But, with indium silicates luminescent material, be prepared into electroluminescent film, have not yet to see report.
Summary of the invention
Based on the problems referred to above, the invention provides a kind of light-emitting film of praseodymium doped indium silicate.
Technical scheme of the present invention is as follows:
The light-emitting film of praseodymium doped indium silicate provided by the invention, its chemical general formula is: MeIn
2-xsi
2o
8: xPr
3+; Wherein, MeIn
2-xsi
2o
8matrix, Pr
3+be exciting light ion, in film, serve as main luminescence center, the value 0.01～0.05 of x, preferably 0.02, Me is selected from Mg, Ca, Sr or Ba element.
The present invention also provides the preparation method of the light-emitting film of above-mentioned praseodymium doped indium silicate, and it utilizes pulsed laser deposition (PLD) to prepare, and processing step is as follows:
(1), the preparation of ceramic target: take respectively MeO, In
2o
3, SiO
2and Pr
2o
3powder, after evenly mixing, sintering at 900～1300 ℃, makes ceramic target, wherein, MeO, In
2o
3, SiO
2and Pr
2o
3mol ratio be 1:1-x/2:2:x/2;
Preferably, ceramic target is cut, its specification is Φ 50 * 2mm; Preferably 1250 ℃ of sintering temperatures.
(2), the ceramic target making and ito glass substrate are packed in the cavity of filming equipment, after enclosed housing, cavity is vacuumized to processing, controlling cavity vacuum tightness is 1.0 * 10
-3pa～1.0 * 10
-5pa;
Preferably, ito glass substrate needs clean before putting into cavity: 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, and then put into vacuum cavity;
Vacuumizing to process adopts mechanical pump and molecular pump that cavity is carried out; Chamber vacuum degree is 5.0 * 10
-4pa.
(3), coating process parameter is set: it is 45～95mm that base target spacing is set, and underlayer temperature is 250 ℃～750 ℃, and in process, passing into flow is the argon gas working gas of 10～35sccm, and operating pressure is 0.2～4Pa; After processing parameter setting completes, carry out coating film treatment, obtain sample, subsequently sample is placed in to anneal 1～3h at 500～800 ℃ of 0.01Pa vacuum ovens; On the ITO of ito glass substrate layer surface, make subsequently the light-emitting film of praseodymium doped indium silicate, its chemical general formula of this light-emitting film is: MeIn
2-xsi
2o
8: xPr
3+; Wherein, MeIn
2-xsi
2o
8matrix, Pr
3+being exciting light ion, is the luminescence center of light-emitting film, and Me is selected from Mg, Ca, and Sr or Ba element, the span of x is 0.01～0.05;
Preferably, coating process parameter is: base target spacing is 60mm, and underlayer temperature is 500 ℃, and in process, passing into flow is the argon gas working gas of 20sccm, and operating pressure is 3Pa, and annealing temperature is 600 ℃, and annealing time is 2h; And the value of x is 0.02.
The present invention also provides a kind of electroluminescent device, comprises glass substrate, ito anode, light-emitting film layer and Ag cathode layer, and wherein, described light-emitting film is the light-emitting film of praseodymium doped indium silicate, and its chemical general formula is: MeIn
2-xsi
2o
8: xPr
3+; Wherein, MeIn
2-xsi
2o
8matrix, Pr
3+being exciting light ion, is the luminescence center of light-emitting film, and Me is selected from Mg, Ca, and Sr or Ba element, the span of x is 0.01～0.05.
The preparation technology of electroluminescent device is as follows:
(1), the preparation of ceramic target: take respectively MeO, In
2o
3, SiO
2and Pr
2o
3powder, after evenly mixing, sintering at 900～1300 ℃, makes ceramic target, wherein, MeO, In
2o
3, SiO
2and Pr
2o
3mol ratio be 1:1-x/2:2:x/2;
(2), the ceramic target making and ito glass substrate are packed in the cavity of filming equipment, after enclosed housing, cavity is vacuumized to processing, controlling cavity vacuum tightness is 1.0 * 10
-3pa～1.0 * 10
-5pa;
(3), coating process parameter is set: it is 45～95mm that base target spacing is set, and underlayer temperature is 250 ℃～750 ℃, and in process, passing into flow is the argon gas working gas of 10～35sccm, and operating pressure is 0.2～4Pa; After processing parameter setting completes, carry out coating film treatment, obtain sample, subsequently sample is placed in to anneal 1～3h at 500～800 ℃ of 0.01Pa vacuum ovens; On the ITO of ito glass substrate layer surface, make subsequently the light-emitting film of praseodymium doped indium silicate, its chemical general formula of this light-emitting film is: MeIn
2-xsi
2o
8: xPr
3+; Wherein, MeIn
2-xsi
2o
8matrix, Pr
3+being exciting light ion, is the luminescence center of light-emitting film, and Me is selected from Mg, Ca, and Sr or Ba element, the span of x is 0.01～0.05;
(4), step (3) makes containing the ito glass substrate of light-emitting film and Ag nanoparticle and moves in vacuum evaporation equipment, plays the Ag layer of cathodic process at light-emitting film surface evaporation one deck;
After above-mentioned steps completes, make electroluminescent device.
The present invention adopts pulsed laser deposition (PLD), prepares praseodymium doped indium silicate light-emitting film, and obtaining, in the electroluminescence spectrum (EL) of film, has very strong glow peak in 625nm position.
Accompanying drawing explanation
Fig. 1 is the EL spectrogram of the light-emitting film sample that makes of embodiment 3;
Fig. 2 is the EL device structure schematic diagram that embodiment 12 makes.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
Select MgO, In
2o
3, SiO
2and Pr
2o
3powder, its mol ratio is 1:0.99:2:0.01, after even mixing, sinters the ceramic target of Φ 50 * 2mm at 1250 ℃ into, 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 3Pa, and underlayer temperature is 500 ℃, and laser energy is 150W, obtains sample MgIn
1.98si
2o
8: 0.02Pr
3+light-emitting film.
Embodiment 2
Select MgO, In
2o
3, SiO
2and Pr
2o
3powder, its mol ratio is 1:0.975:2:0.025, after even mixing, sinters the ceramic target of Φ 50 * 2mm at 900 ℃ into, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 ℃, and laser energy is 80W, obtains sample MgIn
1.95si
2o
8: 0.05Pr
3+light-emitting film.
Embodiment 3
Select MgO, In
2o
3, SiO
2and Pr
2o
3powder, its mol ratio is 1:0.995:2:0.005, after even mixing, sinters the ceramic target of Φ 50 * 2mm at 1300 ℃ into, 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 5Pa, and underlayer temperature is 750 ℃, and laser energy is 300W, obtains sample MgIn
1.99si
2o
8: 0.01Pr
3+light-emitting film.
Fig. 1 is the EL spectrogram of the light-emitting film sample that makes of embodiment 3; As can be seen from Figure 1, in 625nm position, there is very strong glow peak.
Embodiment 4
Select CaO, In
2o
3, SiO
2and Pr
2o
3powder, its mol ratio is 1:0.99:2:0.01, after even mixing, sinters the ceramic target of Φ 50 * 2mm at 1250 ℃ into, 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 3Pa, and underlayer temperature is 500 ℃, and laser energy is 150W, obtains sample CaIn
1.98si
2o
8: 0.02Pr
3+light-emitting film.
Embodiment 5
Select CaO, In
2o
3, SiO
2and Pr
2o
3powder, its mol ratio is 1:0.975:2:0.025, after even mixing, sinters the ceramic target of Φ 50 * 2mm at 900 ℃ into, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 ℃, and laser energy is 80W, obtains sample CaIn
1.95si
2o
8: 0.05Pr
3+light-emitting film.
Embodiment 6
Select MgO, P
2o
5, H
3bO
3, CeO
2and Tb
4o
7powder, its mol ratio is 1:0.995:2:0.005, after even mixing, sinters the ceramic target of Φ 50 * 2mm at 1300 ℃ into, 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 5Pa, and underlayer temperature is 750 ℃, and laser energy is 300W, obtains sample CaIn
1.99si
2o
8: 0.01Pr
3+light-emitting film.
Embodiment 7
Select SrO, In
2o
3, SiO
2and Pr
2o
3powder, its mol ratio is 1:0.99:2:0.01, after even mixing, sinters the ceramic target of Φ 50 * 2mm at 1250 ℃ into, 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 3Pa, and underlayer temperature is 500 ℃, and laser energy is 150W, obtains sample SrIn
1.98si
2o
8: 0.02Pr
3+light-emitting film.
Embodiment 8
Select SrO, In
2o
3, SiO
2and Pr
2o
3powder, its mol ratio is 1:0.975:2:0.025, after even mixing, sinters the ceramic target of Φ 50 * 2mm at 900 ℃ into, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 ℃, and laser energy is 80W, obtains sample SrIn
1.95si
2o
8: 0.05Pr
3+light-emitting film.
Embodiment 9
Select SrO, In
2o
3, SiO
2and Pr
2o
3powder, its mol ratio is 1:0.995:2:0.005, after even mixing, sinters the ceramic target of Φ 50 * 2mm at 1300 ℃ into, 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 5Pa, and underlayer temperature is 750 ℃, and laser energy is 300W, obtains sample SrIn
1.99si
2o
8: 0.01Pr
3+light-emitting film.
Embodiment 10
Select BaO, In
2o
3, SiO
2and Pr
2o
3powder, its mol ratio is 1:0.99:2:0.01, after even mixing, sinters the ceramic target of Φ 50 * 2mm at 1250 ℃ into, 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 3Pa, and underlayer temperature is 500 ℃, and laser energy is 150W, obtains sample BaIn
1.98si
2o
8: 0.02Pr
3+light-emitting film.
Embodiment 11
Select BaO, In
2o
3, SiO
2and Pr
2o
3powder, its mol ratio is 1:0.975:2:0.025, after even mixing, sinters the ceramic target of Φ 50 * 2mm at 900 ℃ into, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 ℃, and laser energy is 80W, obtains sample BaIn
1.95si
2o
8: 0.05Pr
3+light-emitting film.
Embodiment 12
Originally be embodied as electroluminescent device, as shown in Figure 2, wherein, 1 is glass substrate; 2 is ITO transparent conductive film, as anode; 3 is luminescent material thin-film layer; 4 is Ag layer, as negative electrode.
Select BaO, In
2o
3, SiO
2and Pr
2o
3powder, its mol ratio is 1:0.995:2:0.005, after even mixing, sinters the ceramic target of Φ 50 * 2mm at 1300 ℃ into, 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 5Pa, and underlayer temperature is 750 ℃, and laser energy is 300W, obtains sample BaIn
1.99si
2o
8: 0.01Pr
3+light-emitting film.Then light-emitting film is being moved in vacuum evaporation equipment, evaporation one deck Ag on light-emitting film, as negative electrode.
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.
Claims (10)
1. a light-emitting film for praseodymium doped indium silicate, is characterized in that, its chemical general formula is: MeIn
2-xsi
2o
8: xPr
3+; Wherein, MeIn
2-xsi
2o
8matrix, Pr
3+being exciting light ion, is the luminescence center of light-emitting film, and Me is selected from Mg, Ca, and Sr or Ba element, the span of x is 0.01～0.05.
2. the light-emitting film of praseodymium doped indium silicate according to claim 1, is characterized in that, the value of x is 0.02.
3. the light-emitting film of praseodymium doped indium silicate according to claim 1, is characterized in that, comprises the light-emitting film of following chemical formula:
MgIn
1.98Si
2O
8:0.02Pr
3+；MgIn
1.95Si
2O
8:0.05Pr
3+；MgIn
1.99Si
2O
8:0.01Pr
3+；CaIn
1.98Si
2O
8:0.02Pr
3+；CaIn
1.95Si
2O
8:0.05Pr
3+；CaIn
1.99Si
2O
8:0.01Pr
3+；SrIn
1.98Si
2O
8:0.02Pr
3+；SrIn
1.95Si
2O
8:0.05Pr
3+；SrIn
1.99Si
2O
8:0.01Pr
3+；BaIn
1.98Si
2O
8:0.02Pr
3+；BaIn
1.95Si
2O
8:0.05Pr
3+；BaIn
1.99Si
2O
8:0.01Pr
3+。
4. a preparation method for the light-emitting film of praseodymium doped indium silicate, is characterized in that, comprises the steps:
The preparation of ceramic target: take respectively MeO, In
2o
3, SiO
2and Pr
2o
3powder, after evenly mixing, sintering at 900～1300 ℃, makes ceramic target, wherein, MeO, In
2o
3, SiO
2and Pr
2o
3mol ratio be 1:1-x/2:2:x/2;
The ceramic target making and ito glass substrate are packed in the cavity of filming equipment, after enclosed housing, cavity is vacuumized to processing, controlling cavity vacuum tightness is 1.0 * 10
-3pa～1.0 * 10
-5pa;
Coating process parameter is set: it is 45～95mm that base target spacing is set, and underlayer temperature is 250 ℃～750 ℃, in process, passing into flow is the argon gas working gas of 10～35sccm, and operating pressure is 0.2～4Pa; After processing parameter setting completes, carry out coating film treatment, obtain sample, subsequently sample is placed in to anneal 1～3h at 500～800 ℃ of 0.01Pa vacuum ovens; On the ITO of ito glass substrate layer surface, make subsequently the light-emitting film of praseodymium doped indium silicate, its chemical general formula of this light-emitting film is: MeIn
2-xsi
2o
8: xPr
3+; Wherein, MeIn
2-xsi
2o
8matrix, Pr
3+being exciting light ion, is the luminescence center of light-emitting film, and Me is selected from Mg, Ca, and Sr or Ba element, the span of x is 0.01～0.05.
5. the preparation method of the light-emitting film of praseodymium doped indium silicate according to claim 4, is characterized in that, the sintering temperature in described ceramic target preparation process is 1250 ℃.
6. the preparation method of the light-emitting film of praseodymium doped indium silicate according to claim 4, is characterized in that, described in vacuumize and process to adopt mechanical pump and molecular pump that cavity is carried out.
7. the preparation method of the light-emitting film of praseodymium doped indium silicate according to claim 4, is characterized in that, described chamber vacuum degree is 5.0 * 10
-4pa.
8. the preparation method of the light-emitting film of praseodymium doped indium silicate according to claim 4, it is characterized in that, described coating process parameter is: base target spacing is 60mm, underlayer temperature is 500 ℃, in process, passing into flow is the argon gas working gas of 20sccm, operating pressure is 3Pa, and annealing temperature is 600 ℃, and annealing time is 2h.
9. the preparation method of the light-emitting film of praseodymium doped indium silicate according to claim 4, is characterized in that, the value of x is 0.02.
10. an electroluminescent device, comprises glass substrate, ito anode, light-emitting film layer and Ag cathode layer, it is characterized in that, described light-emitting film is the light-emitting film of praseodymium doped indium silicate, and its chemical general formula is: MeIn
2-xsi
2o
8: xPr
3+; Wherein, MeIn
2-xsi
2o
8matrix, Pr
3+being exciting light ion, is the luminescence center of light-emitting film, and Me is selected from Mg, Ca, and Sr or Ba element, the span of x is 0.01～0.05.
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105568219A (en) * | 2015-12-30 | 2016-05-11 | 哈尔滨工业大学 | Preparation method of praseodymium doped potassium-sodium niobate film and application thereof |
| CN109942004A (en) * | 2019-04-10 | 2019-06-28 | 宁波大学 | A kind of strontium silicate magnesium nano material and preparation method thereof and purposes |
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| CN102863954A (en) * | 2011-07-08 | 2013-01-09 | 海洋王照明科技股份有限公司 | Europium-doped calcium silicate luminescent material and preparation method and application thereof |
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2013
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105568219A (en) * | 2015-12-30 | 2016-05-11 | 哈尔滨工业大学 | Preparation method of praseodymium doped potassium-sodium niobate film and application thereof |
| CN105568219B (en) * | 2015-12-30 | 2018-07-03 | 哈尔滨工业大学 | A kind of preparation method and applications of praseodymium doped potassium sodium niobate film |
| CN109942004A (en) * | 2019-04-10 | 2019-06-28 | 宁波大学 | A kind of strontium silicate magnesium nano material and preparation method thereof and purposes |
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Application publication date: 20141203 |