CN104178726A - Luminescent film of antimony-terbium co-doped rare earth aluminoborate and preparation method thereof and electroluminescent device - Google Patents
Luminescent film of antimony-terbium co-doped rare earth aluminoborate and preparation method thereof and electroluminescent device Download PDFInfo
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Abstract
The invention belongs to the photoelectric material field, and discloses a luminescent film of antimony-terbium co-doped rare earth aluminoborate and a preparation method thereof and an electroluminescent device. The general formula of the luminescent film is RAl3(BO3)4:xSb<3+>, yTb<3+>, wherein RAl3(BO3)4 is the matrix, Sb<3+> and Tb<3+>are active photoions and are the luminescence center of the luminescent film, R is selected from Y, La, Gb or Lu, x ranges from 0.01 to 0.05, and y ranges from 0.01 to 0.08. The luminescent film of antimony-terbium co-doped rare earth aluminoborate has a strong luminescence peak at 470 nm and 580 nm in the electroluminescence spectra (EL).
Description
Technical field
The present invention relates to field of photovoltaic materials, relate in particular to light-emitting film of a kind of antimony terbium codoped rare earth-boron aluminate and preparation method thereof.The invention still further relates to a kind of electroluminescent device of this light-emitting film as luminescent layer that use.
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.
The green powder of boron aluminate or phosphate system because its synthesis temperature is moderate, luminosity is high, chromaticity coordinates X value is compared with greatly extremely investigator's favor, is the popular research material of LED fluorescent material.But due to all at high temperature reactions of preparation of material, have like this phosphorus oxide evaporation, cause the ratio of phosphate radical and rare earth element uncontrollable.The development of rare earth-boron aluminate, exactly for overcoming above-mentioned shortcoming.
Summary of the invention
Based on the problems referred to above, the present invention utilizes pulsed laser deposition (PLD), and a kind of preparation method of light-emitting film of antimony terbium codoped rare earth-boron aluminate is provided.
Technical scheme of the present invention is as follows:
A preparation method for the light-emitting film of antimony terbium codoped rare earth-boron aluminate, processing step is as follows:
(1), the preparation of ceramic target: take respectively R
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, after evenly mixing, sintering at 900～1300 DEG C, makes ceramic target, wherein, R
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7mol ratio be 0.5:1.5:2:x:0.25y;
Preferably, ceramic target is cut, its specification is Φ 50 × 2mm; Preferably 1250 DEG C 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 putting into before 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 DEG C～750 DEG C, and the energy of plated film laser is 80～300W, passes into the oxygen that flow is 10～40sccm in process, and operating pressure is 0.5～5Pa; After processing parameter setting completes, carry out coating film treatment; The light-emitting film that makes subsequently antimony terbium codoped rare earth-boron aluminate on the ITO of ito glass substrate layer surface, its chemical general formula of this light-emitting film is: RAl
3(BO
3)
4: xSb
3+, yTb
3+; Wherein, RAl
3(BO
3)
4matrix, Sb
3+and Tb
3+exciting light ion, is the luminescence center of light-emitting film, and R is selected from Y, La, and Gd or Lu element, the span that the span of x is 0.01～0.05, y is 0.01～0.08; Sb
3+excite near the gold-tinted radiation of 580nm, and Tb
3+excite near the blue ray radiation of 470nm; The effect of oxygen is the oxygen element running off in plated film preparation process target in order to compensate, and reduces the radiationless deathnium that oxygen room forms, and increases luminous efficiency;
Preferably, coating process parameter is: base target spacing is 60mm, and underlayer temperature is 500 DEG C, and the energy of plated film laser is 150W, passes into the oxygen that flow is 20sccm in process, and operating pressure is 3Pa; And the value that the value of x is 0.02, y is 0.04.
The present invention also provides a kind of light-emitting film that adopts the antimony terbium codoped rare earth-boron aluminate that aforesaid method makes, and its chemical general formula is: RAl
3(BO
3)
4: xSb
3+, yTb
3+; Wherein, RAl
3(BO
3)
4matrix, Sb
3+and Tb
3+exciting light ion, is the luminescence center of light-emitting film, and R is selected from Y, La, and Gd or Lu element, the span that the span of x is 0.01～0.05, y is 0.01～0.08.
The present invention also provides a kind of electroluminescent device, comprises glass substrate, ito anode, light-emitting film layer and cathode layer, and wherein, described light-emitting film layer is the light-emitting film of antimony terbium codoped rare earth-boron aluminate, and its chemical general formula is: RAl
3(BO
3)
4: xSb
3+, yTb
3+; Wherein, RAl
3(BO
3)
4matrix, Sb
3+and Tb
3+exciting light ion, is the luminescence center of light-emitting film, and R is selected from Y, La, and Gd or Lu element, the span that the span of x is 0.01～0.05, y is 0.01～0.08.
The preparation technology of electroluminescent device is as follows:
(1), the preparation of ceramic target: take respectively R
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, after evenly mixing, sintering at 900～1300 DEG C, makes ceramic target, wherein, R
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7mol ratio be 0.5:1.5:2:x: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 DEG C～750 DEG C, and the energy of plated film laser is 80～300W, passes into the oxygen that flow is 10～40sccm in process, and operating pressure is 0.5～5Pa; After processing parameter setting completes, carry out coating film treatment; The light-emitting film that makes subsequently antimony terbium codoped rare earth-boron aluminate on the ITO of ito glass substrate layer surface, its chemical general formula of this light-emitting film is: RAl
3(BO
3)
4: xSb
3+, yTb
3+; Wherein, RAl
3(BO
3)
4matrix, Sb
3+and Tb
3+exciting light ion, is the luminescence center of light-emitting film, and R is selected from Y, La, and Gd or Lu element, the span that the span of x is 0.01～0.05, y is 0.01～0.08;
(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 PLD equipment, prepares antimony terbium codoped rare earth-boron aluminate light-emitting film, obtains, in the electroluminescence spectrum (EL) of film, having very strong glow peak at 470nm and 580nm position.
Adopt preparation method of the present invention, can prepare dystectic material, and non-conducting material, the thin-film material quality obtaining is good, and the luminous efficiency of making light-emitting film is high.
Brief description of the drawings
Fig. 1 is the EL spectrogram of the light-emitting film sample that makes of embodiment 7;
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
Take Y
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, its mol ratio is 0.5:1.5:2:0.02:0.01, after even mixing, sinters the ceramic target of Φ 50 × 2mm at 1250 DEG C 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.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 20sccm, and pressure is adjusted to 3Pa, and underlayer temperature is 500 DEG C, and laser energy is 150W, obtains sample YAl
3(BO
3)
4: 0.02Sb
3+, 0.04Tb
3+light-emitting film.
Embodiment 2
Take Y
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, its mol ratio is 0.5:1.5:2:0.01:0.02, after even mixing, sinters the ceramic target of Φ 50 × 2mm at 900 DEG C 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 DEG C, and laser energy is 80W, obtains sample YAl
3(BO
3)
4: 0.01Sb
3+, 0.08Tb
3+light-emitting film.
Embodiment 3
Take Y
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, its mol ratio is 0.5:1.5:2:0.05:0.0.0025, after even mixing, sinters the ceramic target of Φ 50 × 2mm at 1300 DEG C 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.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 40sccm, and pressure is adjusted to 5Pa, and underlayer temperature is 750 DEG C, and laser energy is 300W, obtains sample YAl
3(BO
3)
4: 0.05Sb
3+, 0.01Tb
3+light-emitting film.
Embodiment 4
Take La
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, its mol ratio is 0.5:1.5:2:0.02:0.01, after even mixing, sinters the ceramic target of Φ 50 × 2mm at 1250 DEG C 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.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 20sccm, and pressure is adjusted to 3Pa, and underlayer temperature is 500 DEG C, and laser energy is 150W, obtains sample LaAl
3(BO
3)
4: 0.02Sb
3+, 0.04Tb
3+light-emitting film.
Embodiment 5
Take La
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, its mol ratio is 0.5:1.5:2:0.01:0.02, after even mixing, sinters the ceramic target of Φ 50 × 2mm at 900 DEG C 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 DEG C, and laser energy is 80W, obtains sample LaAl
3(BO
3)
4: 0.01Sb
3+, 0.08Tb
3+light-emitting film.
Embodiment 6
Take La
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, its mol ratio is 0.5:1.5:2:0.05:0.0.0025, after even mixing, sinters the ceramic target of Φ 50 × 2mm at 1300 DEG C 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.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 40sccm, and pressure is adjusted to 5Pa, and underlayer temperature is 750 DEG C, and laser energy is 300W, obtains sample LaAl
3(BO
3)
4: 0.05Sb
3+, 0.01Tb
3+light-emitting film.
Embodiment 7
Take Gd
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, its mol ratio is 0.5:1.5:2:0.02:0.01, after even mixing, sinters the ceramic target of Φ 50 × 2mm at 1250 DEG C 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.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 20sccm, and pressure is adjusted to 3Pa, and underlayer temperature is 500 DEG C, and laser energy is 150W, obtains sample GdAl
3(BO
3)
4: 0.02Sb
3+, 0.04Tb
3+light-emitting film.
Fig. 1 is the EL spectrogram of the light-emitting film sample that makes of embodiment 7; As can be seen from Figure 1, there is very strong glow peak at 470nm and 580nm position.
Embodiment 8
Get Gd
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, its mol ratio is 0.5:1.5:2:0.01:0.02, after even mixing, sinters the ceramic target of Φ 50 × 2mm at 900 DEG C 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 DEG C, and laser energy is 80W, obtains sample GdAl
3(BO
3)
4: 0.01Sb
3+, 0.08Tb
3+light-emitting film.
Embodiment 9
Take Gd
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, its mol ratio is 0.5:1.5:2:0.05:0.0.0025, after even mixing, sinters the ceramic target of Φ 50 × 2mm at 1300 DEG C 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.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 40sccm, and pressure is adjusted to 5Pa, and underlayer temperature is 750 DEG C, and laser energy is 300W, obtains sample GdAl
3(BO
3)
4: 0.05Sb
3+, 0.01Tb
3+light-emitting film.
Embodiment 10
Take Lu
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, its mol ratio is 0.5:1.5:2:0.02:0.01, after even mixing, sinters the ceramic target of Φ 50 × 2mm at 1250 DEG C 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.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 20sccm, and pressure is adjusted to 3Pa, and underlayer temperature is 500 DEG C, and laser energy is 150W, obtains sample LuAl
3(BO
3)
4: 0.02Sb
3+, 0.04Tb
3+light-emitting film.
Embodiment 11
Take Lu
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, its mol ratio is 0.5:1.5:2:0.01:0.02, after even mixing, sinters the ceramic target of Φ 50 × 2mm at 900 DEG C 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.The vacuum tightness of cavity is extracted into 1.0 × 10 with mechanical pump and molecular pump
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 DEG C, and laser energy is 80W, obtains sample LuAl
3(BO
3)
4: 0.01Sb
3+, 0.08Tb
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.
Take Lu
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, its mol ratio is 0.5:1.5:2:0.05:0.0.0025, after even mixing, sinters the ceramic target of Φ 50 × 2mm at 1300 DEG C 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.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 40sccm, and pressure is adjusted to 5Pa, and underlayer temperature is 750 DEG C, and laser energy is 300W, obtains sample LuAl
3(BO
3)
4: 0.05Sb
3+, 0.01Tb
3+light-emitting film.Then light-emitting film is 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 preparation method for the light-emitting film of antimony terbium codoped rare earth-boron aluminate, is characterized in that, comprises the steps:
The preparation of ceramic target: take respectively R
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7powder, after evenly mixing, sintering at 900～1300 DEG C, makes ceramic target, wherein, R
2o
3, Al
2o
3, B
2o
3, SbO
2and Tb
4o
7mol ratio be 0.5:1.5:2:x: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 DEG C～750 DEG C, and the energy of plated film laser is 80～300W, passes into the oxygen that flow is 10～40sccm in process, and operating pressure is 0.5～5Pa; After processing parameter setting completes, carry out coating film treatment; The light-emitting film that makes subsequently antimony terbium codoped rare earth-boron aluminate on the ITO of ito glass substrate layer surface, its chemical general formula of this light-emitting film is: RAl
3(BO
3)
4: xSb
3+, yTb
3+; Wherein, RAl
3(BO
3)
4matrix, Sb
3+and Tb
3+exciting light ion, is the luminescence center of light-emitting film, and R is selected from Y, La, and Gd or Lu element, the span that the span of x is 0.01～0.05, y is 0.01～0.08.
2. the preparation method of the light-emitting film of antimony terbium codoped rare earth-boron aluminate according to claim 1, is characterized in that, the sintering temperature in described ceramic target preparation process is 1250 DEG C.
3. the preparation method of the light-emitting film of antimony terbium codoped rare earth-boron aluminate according to claim 1, is characterized in that, described in vacuumize to process and adopt mechanical pump and molecular pump that cavity is carried out.
4. the preparation method of the light-emitting film of antimony terbium codoped rare earth-boron aluminate according to claim 1, it is characterized in that, ito glass substrate needs clean putting into before cavity: successively use acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ito glass substrate, and use it is carried out to oxygen plasma treatment, and then put into vacuum cavity.
5. the preparation method of the light-emitting film of antimony terbium codoped rare earth-boron aluminate according to claim 1, is characterized in that, described chamber vacuum degree is 5.0 × 10
-4pa.
6. the preparation method of the light-emitting film of antimony terbium codoped rare earth-boron aluminate according to claim 1, it is characterized in that, described coating process parameter is: base target spacing is 60mm, underlayer temperature is 500 DEG C, the energy of plated film laser is 150W, in process, pass into the oxygen that flow is 20sccm, operating pressure is 3Pa.
7. the preparation method of the light-emitting film of antimony terbium codoped rare earth-boron aluminate according to claim 1, is characterized in that, the value that the value of x is 0.02, y is 0.04.
8. one kind adopts the light-emitting film of the antimony terbium codoped rare earth-boron aluminate that the arbitrary described preparation method of claim 1 to 7 makes.
9. the light-emitting film of antimony terbium codoped rare earth-boron aluminate according to claim 8, is characterized in that, comprises the light-emitting film of following chemical formula: YAl
3(BO
3)
4: 0.02Sb
3+, 0.04Tb
3+; YAl
3(BO
3)
4: 0.01Sb
3+, 0.08Tb
3+; YAl
3(BO
3)
4: 0.05Sb
3+, 0.01Tb
3+; LaAl
3(BO
3)
4: 0.02Sb
3+, 0.04Tb
3+; LaAl
3(BO
3)
4: 0.01Sb
3+, 0.08Tb
3+; LaAl
3(BO
3)
4: 0.05Sb
3+, 0.01Tb
3+; GdAl
3(BO
3)
4: 0.02Sb
3+, 0.04Tb
3+; GdAl
3(BO
3)
4: 0.01Sb
3+, 0.08Tb
3+; GdAl
3(BO
3)
4: 0.05Sb
3+, 0.01Tb
3+; LuAl
3(BO
3)
4: 0.02Sb
3+, 0.04Tb
3+; LuAl
3(BO
3)
4: 0.01Sb
3+, 0.08Tb
3+; LuAl
3(BO
3)
4: 0.05Sb
3+, 0.01Tb
3+.
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 layer adopts the light-emitting film of antimony terbium codoped rare earth-boron aluminate described in claim 8 or 9.
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Application publication date: 20141203 |