CN104178153A - Europium terbium-doped hafnium oxide-based light-emitting film and preparation method thereof and electroluminescent device - Google Patents
Europium terbium-doped hafnium oxide-based light-emitting film and preparation method thereof and electroluminescent device Download PDFInfo
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- CN104178153A CN104178153A CN201310196683.8A CN201310196683A CN104178153A CN 104178153 A CN104178153 A CN 104178153A CN 201310196683 A CN201310196683 A CN 201310196683A CN 104178153 A CN104178153 A CN 104178153A
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Abstract
The invention belongs to the field of photoelectric materials, and discloses an europium terbium-doped hafnium oxide-based light-emitting film and a preparation method thereof and an electroluminescent device; the light-emitting film has a chemical formula of Hf1-x-yO2:xEu<2 +>, yTb<3 +>; wherein Hf1-x-yO2 is a matrix, Eu<2 +> andTb <3 +> are activated light ions, and are light-emitting centers of the light-emitting film, the value range of x is 0.01-0.05, and the value range of y is 0.005-0.03. In the electroluminescence spectrum (EL) of the europium terbium-doped hafnium oxide-based light-emitting film, strong light-emitting peaks show at 480nm and 580nm positions.
Description
Technical field
The present invention relates to field of photovoltaic materials, relate in particular to light-emitting film of the terbium doped hafnium oxide base of a kind of europium 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.
Hafnia class luminescent material is the popular research material as LED fluorescent material.Burst of ultraviolel blue colour fluorescent powder can be used as commercial product, and is constantly improving in research and development.
Summary of the invention
Based on the problems referred to above, the invention provides the light-emitting film of the terbium doped hafnium oxide base of a kind of europium.
Technical scheme of the present invention is as follows:
The light-emitting film of the terbium doped hafnium oxide base of europium provided by the invention, its chemical general formula is: Hf
1-x-yo
2: xEu
2+, yTb
3+; Wherein, HfO
2matrix, Eu
2+and Tb
3+be exciting light ion, in film, serve as main luminescence center, the value 0.01～0.05 of x, preferably 0.03, y value 0.005～0.03, preferably 0.01; Eu
2+excite near the gold-tinted radiation of 580nm, and Tb
3+excite near the blue ray radiation of 480nm.
The present invention also provides the preparation method of the light-emitting film of the terbium doped hafnium oxide base of above-mentioned europium, and it utilizes magnetron sputtering method to prepare, and processing step is as follows:
(1), the preparation of ceramic target: take respectively HfO
2, Eu
2o
3and Tb
4o
7powder, after evenly mixing, sintering at 900～1300 ℃, makes ceramic target, wherein, HfO
2, Eu
2o
3and Tb
4o
7mol ratio be 1-x-y:0.5x:0.25y;
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 the terbium doped hafnium oxide base of europium, its chemical general formula of this light-emitting film is: Hf
1-x-yo
2: xEu
2+, yTb
3+; Wherein, HfO
2matrix, Eu
2+and Tb
3+being exciting light ion, is the luminescence center of light-emitting film, and the span that the span of x is 0.01～0.05, y is 0.005～0.03;
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 that the value of x is 0.03, y is 0.01.
The present invention also provides a kind of electroluminescent device, comprises glass substrate, ito anode, light-emitting film layer and cathode layer, it is characterized in that, described light-emitting film is the light-emitting film of the terbium doped hafnium oxide base of europium, and its chemical general formula is: Hf
1-x-yo
2: xEu
2+, yTb
3+; Wherein, HfO
2matrix, Eu
2+and Tb
3+being exciting light ion, is the luminescence center of light-emitting film, and the span that the span of x is 0.01～0.05, y is 0.005～0.03.
The preparation technology of electroluminescent device is as follows:
(1), the preparation of ceramic target: take respectively HfO
2, Eu
2o
3and Tb
4o
7powder, after evenly mixing, sintering at 900～1300 ℃, makes ceramic target, wherein, HfO
2, Eu
2o
3and Tb
4o
7mol ratio be 1-x-y:0.5x:0.25y;
(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 the terbium doped hafnium oxide base of europium, its chemical general formula of this light-emitting film is: Hf
1-x-yo
2: xEu
2+, yTb
3+; Wherein, HfO
2matrix, Eu
2+and Tb
3+being exciting light ion, is the luminescence center of light-emitting film, and the span that the span of x is 0.01～0.05, y is 0.005～0.03;
(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 magnetron sputtering equipment, prepares the terbium doped hafnium oxide light-emitting film of europium, and obtaining, in the electroluminescence spectrum (EL) of film, has very strong glow peak at 480nm and 580nm 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 5 makes.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
Select HfO
2, Eu
2o
3and Tb
4o
7powder, its mole number is respectively 0.96mmol, 0.015mmol, 0.0025mmol after even mixing, sinters the ceramic target of Φ 50 * 2mm into, and target is packed in vacuum cavity at 1250 ℃.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 argon gas is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 ℃.The sample the obtaining 2h that anneals in 0.01Pa vacuum oven, annealing temperature is 600 ℃.Obtain sample Hf
0.96o
2: 0.03Eu
2+, 0.01Tb
3+light-emitting film.
Fig. 1 is the EL spectrum of the hafnium oxide light-emitting film that makes of embodiment 1; Obtain, in the electroluminescence spectrum (EL) of film, at 480nm and 580nm position, having very strong glow peak.
Embodiment 2
Select HfO
2, Eu
2o
3and Tb
4o
7powder, its mole number is respectively 0.985mmol, 0.005mmol, 0.00125mmol after even mixing, sinters the ceramic target of Φ 50 * 2mm into, and target is packed in vacuum cavity at 900 ℃.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 argon gas is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 ℃.The sample the obtaining 1h that anneals in 0.01Pa vacuum oven, annealing temperature is 500 ℃.Obtain sample Hf
0.985o
2: 0.01Eu
2+, 0.005Tb
3+light-emitting film.
Embodiment 3
Select HfO
2, Eu
2o
3and Tb
4o
7powder, its mole number is respectively 0.92mmol, 0.025mmol, 0.0075mmol after even mixing, sinters the ceramic target of Φ 50 * 2mm into, and target is packed in vacuum cavity at 1150 ℃.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 argon gas is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 ℃.The sample the obtaining 3h that anneals in 0.01Pa vacuum oven, annealing temperature is 800 ℃.Obtain sample Hf
0.92o
2: 0.05Eu
2+, 0.03Tb
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, at 480nm and 580nm position, there is very strong glow peak.
Embodiment 4
Select HfO
2, Eu
2o
3and Tb
4o
7powder, its mole number is respectively 0.95mmol, 0.02mmol, 0.0025mmol after even mixing, sinters the ceramic target of Φ 50 * 2mm into, and target is packed in vacuum cavity at 1300 ℃.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 55mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 6.0 * 10
-4pa, the working gas flow of argon gas is 15sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 600 ℃.The sample the obtaining 1.5h that anneals in 0.01Pa vacuum oven, annealing temperature is 700 ℃.Obtain sample Hf
0.95o
2: 0.04Eu
2+, 0.01Tb
3+light-emitting film.
Embodiment 5
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 HfO
2, Eu
2o
3and Tb
4o
7powder, its mole number is respectively 0.96mmol, 0.01mmol, 0.005mmol after even mixing, sinters the ceramic target of Φ 50 * 2mm into, and target is packed in vacuum cavity at 950 ℃.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 80mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 3.0 * 10
-4pa, the working gas flow of argon gas is 20sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 650 ℃.The sample the obtaining 2.5h that anneals in 0.01Pa vacuum oven, annealing temperature is 650 ℃.Obtain sample Hf
0.96o
2: 0.02Eu
2+, 0.02Tb
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 the terbium doped hafnium oxide base of europium, is characterized in that, its chemical general formula is: Hf
1-x-yo
2: xEu
2+, yTb
3+; Wherein, HfO
2matrix, Eu
2+and Tb
3+being exciting light ion, is the luminescence center of light-emitting film, and the span that the span of x is 0.01～0.05, y is 0.005～0.03.
2. the light-emitting film of the terbium doped hafnium oxide base of europium according to claim 1, is characterized in that, the value that the value of x is 0.03, y is 0.01.
3. the light-emitting film of the terbium doped hafnium oxide base of europium according to claim 1, is characterized in that, comprises the light-emitting film of following chemical formula:
Hf
0.96O
2:0.03Eu
2+,0.01Tb
3+；Hf
0.985O
2:0.01Eu
2+,0.005Tb
3+；Hf
0.92O
2:0.05Eu
2+,0.03Tb
3+；Hf
0.95O
2:0.04Eu
2+,0.01Tb
3+；Hf
0.96O
2:0.02Eu
2+,0.02Tb
3+。
4. a preparation method for the light-emitting film of the terbium doped hafnium oxide base of europium, is characterized in that, comprises the steps:
The preparation of ceramic target: take respectively HfO
2, Eu
2o
3and Tb
4o
7powder, after evenly mixing, sintering at 900～1300 ℃, makes ceramic target, wherein, HfO
2, Eu
2o
3and Tb
4o
7mol ratio be 1-x-y:0.5x:0.25y;
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 the terbium doped hafnium oxide base of europium, its chemical general formula of this light-emitting film is: Hf
1-x-yo
2: xEu
2+, yTb
3+; Wherein, HfO
2matrix, Eu
2+and Tb
3+being exciting light ion, is the luminescence center of light-emitting film, and the span that the span of x is 0.01～0.05, y is 0.005～0.03.
5. the preparation method of the light-emitting film of the terbium doped hafnium oxide base of europium 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 the terbium doped hafnium oxide base of europium 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 the terbium doped hafnium oxide base of europium 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 the terbium doped hafnium oxide base of europium 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 the terbium doped hafnium oxide base of europium according to claim 4, is characterized in that, the value that the value of x is 0.03, y is 0.01.
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 the terbium doped hafnium oxide base of europium, and its chemical general formula is: Hf
1-x-yo
2: xEu
2+, yTb
3+; Wherein, HfO
2matrix, Eu
2+and Tb
3+being exciting light ion, is the luminescence center of light-emitting film, and the span that the span of x is 0.01～0.05, y is 0.005～0.03.
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Cited By (1)
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| CN109321008A (en) * | 2018-12-12 | 2019-02-12 | 郴州市泰益表面涂层技术有限公司 | Superhigh temperature high emissivity infrared radiating coating and preparation method thereof |
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| CN109321008A (en) * | 2018-12-12 | 2019-02-12 | 郴州市泰益表面涂层技术有限公司 | Superhigh temperature high emissivity infrared radiating coating and preparation method thereof |
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Application publication date: 20141203 |