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CN102911666B - Cerium-tin-codoped strontium chlorophosphate light-emitting film and preparation method thereof, and organic electroluminescent device - Google Patents

Cerium-tin-codoped strontium chlorophosphate light-emitting film and preparation method thereof, and organic electroluminescent device Download PDF

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CN102911666B
CN102911666B CN201110224340.9A CN201110224340A CN102911666B CN 102911666 B CN102911666 B CN 102911666B CN 201110224340 A CN201110224340 A CN 201110224340A CN 102911666 B CN102911666 B CN 102911666B
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emitting film
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CN102911666A (en
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周明杰
王平
陈吉星
黄辉
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

The invention belongs to the field of electroluminescent films, and discloses a cerium-tin-codoped strontium chlorophosphate light-emitting film and a preparation method thereof, and an organic electroluminescent device. The chemical general formula of the light-emitting film is Sr5(PO4)3Clx:mCe<3+>,nSn<4+>, wherein Sr5(PO4)3Clx is the matrix, and Ce<3+> and Sn4<+> are doping elements; and x is 0.8-1.2, m is 0.001-0.027, and n is 0.001-0.050. A magnetron sputtering device is utilized to prepare the cerium-tin-codoped strontium chlorophosphate light-emitting film; and the cerium-tin-codoped strontium chlorophosphate light-emitting film has strong light-emitting peaks in the wavelength regions of 450nm and 480nm, and is a developing material for electroluminescent devices.

Description

Cerium tin codoped chlorine strontium phosphate light-emitting film, its preparation method and organic electroluminescence device
Technical field
The present invention relates to photo-electroluminescence film field, relate in particular to a kind of cerium tin codoped chlorine strontium phosphate light-emitting film and preparation method thereof.The invention still further relates to a kind of this cerium tin codoped chlorine strontium phosphate light-emitting film that uses as the organic electroluminescence device of luminescent layer.
Background technology
Compare with the display screen that traditional luminescent powder is made, light-emitting film contrast gradient, resolving power, thermal conduction, homogeneity, and the aspect such as the tack of substrate, outgas speed all demonstrate stronger superiority.Therefore,, as functional materials, light-emitting film has broad application prospects in electroluminescent device (TFELD) flat pannel display field.
Alkaline-earth metal halide phosphate is the luminous host material that a class is very important, study morely.Rare-earth ion activated alkaline earth chlorophosphate is a class blue light-emitting and efficiency light electroluminescent material blue green light, excellent property that development in recent years is got up, and as red-green glow fluorescent material, is widely used in electroluminescent device production.But, with alkaline-earth metal halide phosphate class luminescent material, be prepared into electroluminescent film, still rarely seen report.
Summary of the invention
The object of the invention is to provide a kind of cerium tin codoped chlorine strontium phosphate light-emitting film that chlorine strontium phosphate is main luminescence center as matrix, cerium and tin element of take.
Cerium tin codoped chlorine strontium phosphate light-emitting film of the present invention, the chemical general formula of film is Sr 5(PO 4) 3cl x: mCe 3+, nSn 4+; Wherein, Sr 5(PO 4) 3cl xfor matrix, Ce 3+and Sn 4+for doped element; The span of x is that 0.8～1.2, m span is that 0.001～0.027, n span is 0.001～0.050; Preferably the value of x is that 1, m span is that 0.006, n span is 0.018.
Another goal of the invention of the present invention is to provide the preparation method of above-mentioned cerium tin codoped chlorine strontium phosphate light-emitting film, and its preparation technology is as follows:
The preparation of step S1, ceramic target: according to chemical general formula Sr 5(PO 4) 3cl x: mCe 3+, nSn 4+in each element chemistry metering ratio, select SrO, SrCl 2, P 2o 5, CeO 2and SnO 2powder, after even mixing, at 900～1300 ℃ (preferably 1250 ℃) lower sintering, obtains target; Wherein, the span of x is that 0.8～1.2, m span is that 0.001～0.027, n span is 0.001～0.050; Preferably the value of x is that 1, m span is that 0.006, n span is 0.018.
Step S2, the target in step S1 and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, with mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 * 10 -3pa～1.0 * 10 -5pa, preferably vacuum tightness is 5.0 * 10 -4pa;
Step S3, adjustment magnetron sputtering plating processing parameter are: base target spacing is 45～90mm, preferably 60mm; Underlayer temperature is 250 ℃～750 ℃, preferably 500 ℃; Gas flow 10～the 35sccm of argon gas working gas, preferably 25sccm; Magnetron sputtering operating pressure 0.2～4Pa, preferably 2.0Pa; After processing parameter has been adjusted, be then filmed, obtain film sample;
Step S4, the film sample that step S3 is obtained are placed in vacuum oven, (being 0.01Pa) anneal 1～3h under 500～800 ℃ (preferably 600 ℃), vacuum state (preferably 2h), and obtaining chemical general formula is Sr 5(PO 4) 3cl x: mCe 3+, nSn 4+cerium tin codoped chlorine strontium phosphate light-emitting film; Wherein, Sr 5(PO 4) 3cl xfor matrix, Ce 3+and Sn 4+for doped element.
The present invention also provides a kind of organic electroluminescence device, and this device is straticulate structure, and this straticulate structure is followed successively by substrate, anode layer, luminescent layer and cathode layer; Wherein, luminescent layer is that (chemical general formula of this light-emitting film is Sr to cerium tin codoped chlorine strontium phosphate light-emitting film 5(PO 4) 3cl x: mCe 3+, nSn 4+; Wherein, Sr 5(PO 4) 3cl xfor matrix, Ce 3+and Sn 4+for doped element; The span of x is that 0.8～1.2, m span is that 0.001～0.027, n span is 0.001～0.050; Preferably the value of x is that 1, m span is that 0.006, n span is 0.018), substrate is glass, and anode layer is ITO, and cathode layer is Ag layer, and Ag layer adopts evaporation process preparation at film surface.
The present invention adopts magnetron sputtering equipment, prepares cerium tin codoped chlorine strontium phosphate light-emitting film, obtains, in the electroluminescent spectrum (EL) of film, at 450nm and 480nm wavelength zone, having very strong glow peak, is the development material of electroluminescent device.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of cerium tin codoped chlorine strontium phosphate light-emitting film of the present invention;
Fig. 2 is the structural representation of organic electroluminescence device of the present invention;
Fig. 3 is the electroluminescent spectrum that embodiment 4 obtains cerium tin codoped chlorine strontium phosphate light-emitting film.
Embodiment
A kind of cerium tin codoped chlorine strontium phosphate light-emitting film provided by the invention, it is Sr that this cerium tin codoped chlorine strontium phosphate light-emitting film comprises film general formula 5(PO 4) 3cl x: mCe 3+, nSn 4+; Wherein, Sr 5(PO 4) 3cl xfor matrix, Ce 3+and Sn 4+for doped element, be also active element, and serve as main luminescence center; The span of x is that 0.8～1.2, m span is that 0.001～0.027, n span is 0.001～0.050; The value that the value that preferably value of x is 1, m is 0.006, n is 0.018.
Above-mentioned cerium tin codoped chlorine strontium phosphate light-emitting film preparation method, as shown in Figure 1, its preparation technology is as follows:
The preparation of step S1, ceramic target: according to chemical general formula Sr 5(PO 4) 3cl x: mCe 3+, nSn 4+in each element chemistry metering ratio, select SrO, SrCl 2, P 2o 5, CeO 2and SnO 2powder, after even mixing, at 900～1300 ℃ (preferably 1250 ℃) lower sintering, naturally cooling, obtains target sample, and it is the target that 50mm, thickness are 2mm that target sample is cut into diameter; Wherein, the span of x is that 0.8～1.2, m span is that 0.001～0.027, n span is 0.001～0.050, and preferably the value of x is that 1, m span is that 0.006, n span is 0.018;
Step S2, the target in step S1 and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, with mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 * 10 -3pa～1.0 * 10 -5pa, preferably 5.0 * 10 -4pa;
Step S3, adjustment magnetron sputtering plating processing parameter are: base target spacing is 45～90mm, preferably 60mm; Underlayer temperature is 250 ℃～750 ℃, preferably 500 ℃; Gas flow 10～the 35sccm of argon gas working gas, preferably 25sccm; Magnetron sputtering operating pressure 0.2～4Pa, preferably 2.0Pa; Processing parameter is then filmed after adjusting, and obtains film sample;
Step S4, the film sample that step S3 is obtained are placed in vacuum oven, (being 0.01Pa) anneal 1～3h under 500～800 ℃ (preferably 600 ℃), vacuum state (preferably 2h), and obtaining chemical general formula is Sr 5(PO 4) 3cl x: mCe 3+, nSn 4+described cerium tin codoped chlorine strontium phosphate light-emitting film; Wherein, Sr 5(PO 4) 3cl xfor matrix, Ce 3+and Sn 4+for doped element.
In above-mentioned preparation method step S1, according to chemical general formula Sr 5(PO 4) 3cl x: mCe 3+, nSn 4+(wherein, the span of x is that 0.8～1.2, m span is 0.001～0.027, n span is 0.001～0.050, and preferably the value of x is that 1, m span is 0.006, n span is 0.018) in each element chemistry metering ratio, actual SrO, the SrCl of weighing 2, P 2o 5, Ce 2o 3and SnO 2during powder, by mass percentage: SrO account for total amount 55～70%, P 2o 5account for total amount 23～30%, SrCl 2account for total amount 5～15%, Ce 2o 3account for total amount 0.1～3%, SnO 2account for 0.1～5% of total amount; Preferably, SrO account for total amount 62.5%, P 2o 5account for total amount 27%, SrCl 2account for total amount 8%, Ce 2o 3account for total amount 0.7%, SnO 2account for 1.8% of total amount.
The present invention also provides a kind of organic electroluminescence device, and as shown in Figure 2, this device is straticulate structure, and this straticulate structure is followed successively by substrate 1, anode layer 2, luminescent layer 3 and cathode layer 4; Wherein, substrate 1 is glass, and anode layer 2 is ITO layer, and ito glass, can buy acquisition; For cerium tin codoped chlorine strontium phosphate light-emitting film layer, (chemical general formula of this light-emitting film is Sr to luminescent layer 3 5(PO 4) 3cl x: mCe 3+, nSn 4+; Wherein, Sr 5(PO 4) 3cl xfor matrix, Ce 3+and Sn 4+for doped element; The span of x is 0.8～1.2, m span is 0.001～0.027, n span is 0.001～0.050, preferably the value of x is that 1, m span is that 0.006, n span is 0.018), substrate 1 is glass, anode layer 2 is ITO, and cathode layer 4 is Ag layer, and Ag layer adopts evaporation process preparation at film surface.
The present invention adopts magnetron sputtering equipment, prepares cerium tin codoped chlorine strontium phosphate light-emitting film, obtains, in the electroluminescent spectrum (EL) of film, at 450nm and 480nm wavelength zone, having very strong glow peak, is the development material of electroluminescent device.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
1, select purity to be respectively 99.99% SrO, SrCl 2, P 2o 5, Ce 2o 3and SnO 2powder, according to mass percent: SrO～62.5%, SrCl 2～8%, Ce 2o 3～0.7%, SnO 2～1.8% and P 2o 5～27%, take SrO, SrCl 2, P 2o 5, Ce 2o 3and SnO 2the total mass number of powder is respectively 12.5g, 1.6g, 0.14g, 0.36g, 5.4g; These powders after even mixing, sintering at 1250 ℃, naturally cooling, obtains target sample, it is the target that 50mm, thickness are 2mm that target sample is cut into diameter;
2, target is packed in the vacuum cavity of magnetic-controlled sputtering coating equipment;
3, successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass, and it is carried out to oxygen plasma treatment, put into the vacuum cavity of magnetic-controlled sputtering coating equipment after complete; Wherein, the base target spacing setting of target and glass is 60mm;
4, with mechanical pump and molecular pump, the vacuum tightness of the vacuum cavity of magnetic-controlled sputtering coating equipment is extracted into 5.0 * 10 -4pa;
5, adjust magnetron sputtering plating processing parameter: argon gas working gas flow is 25sccm; Magnetron sputtering operating pressure is 2.0Pa; Underlayer temperature is 500 ℃; Then be filmed the film sample obtaining;
6, film sample is annealed in 0.01Pa vacuum oven 2h, annealing temperature is 600 ℃, obtains cerium tin codoped chlorine strontium phosphate light-emitting film, i.e. Sr 5(PO 4) 3cl:0.006Ce 3+, 0.018Sn 4+.
Embodiment 2
1,, select purity to be respectively 99.99% SrO, SrCl 2, P 2o 5, Ce 2o 3and SnO 2powder, according to mass percent: SrO～56.9%, SrCl 2～15%, Ce 2o 3～0.1%, SnO 2～5% and P 2o 5～23%, take SrO, SrCl 2, P 2o 5, Ce 2o 3and SnO 2the total mass number of powder is respectively 11.38g, 3g, 0.2g, 1g, 4.6g; These powders after even mixing, sintering at 900 ℃, naturally cooling, obtains target sample, it is the target that 50mm, thickness are 2mm that target sample is cut into diameter;
2, target is packed in the vacuum cavity of magnetic-controlled sputtering coating equipment;
3, successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass, and it is carried out to oxygen plasma treatment, put into the vacuum cavity of magnetic-controlled sputtering coating equipment after complete; Wherein, the base target spacing setting of target and glass is 45mm;
4, with mechanical pump and molecular pump, the vacuum tightness of the vacuum cavity of magnetic-controlled sputtering coating equipment is extracted into 1.0 * 10 -3pa;
5, adjust magnetron sputtering plating processing parameter: argon gas working gas flow is 10sccm; Magnetron sputtering operating pressure is 4Pa; Underlayer temperature is 250 ℃; Then be filmed the film sample obtaining;
6, film sample is annealed in 0.01Pa vacuum oven 1h, annealing temperature is 500 ℃, obtains cerium tin codoped chlorine strontium phosphate light-emitting film, i.e. Sr 5(PO 4) 3cl 1.2: 0.001Ce 3+, 0.050Sn 4+.
Embodiment 3
1, select purity to be respectively 99.99% SrO, SrCl 2, P 2o 5, Ce 2o 3and SnO 2powder, according to mass percent: SrO～70%, SrCl 2～5%, Ce 2o 3～3% He, SnO 2～0.1%, P 2o 5～21.9%, take SrO, SrCl 2, P 2o 5, CeO 2and SnO 2the total mass number of powder is respectively 14g, 1g, 0.6g, 0.02g, 4.38g; These powders after even mixing, sintering at 1300 ℃, naturally cooling, obtains target sample, it is the target that 50mm, thickness are 2mm that target sample is cut into diameter;
2, target is packed in the vacuum cavity of magnetic-controlled sputtering coating equipment;
3, successively by acetone, dehydrated alcohol and deionized water ultrasonic cleaning band glass substrate, and it is carried out to oxygen plasma treatment, put into the vacuum cavity of magnetic-controlled sputtering coating equipment after complete; Wherein, the base target spacing setting of target and glass is 90mm;
4, with mechanical pump and molecular pump, the vacuum tightness of the vacuum cavity of magnetic-controlled sputtering coating equipment is extracted into 1.0 * 10 -5pa;
5, adjust magnetron sputtering plating processing parameter: argon gas working gas flow is 35sccm; Magnetron sputtering operating pressure is 0.2Pa; Underlayer temperature is 750 ℃; Then be filmed the film sample obtaining;
6, film sample is annealed in 0.01Pa vacuum oven 3h, annealing temperature is 800 ℃, obtains cerium tin codoped chlorine strontium phosphate light-emitting film, i.e. Sr 5(PO 4) 3cl 0.8: 0.027Ce 3+, 0.001Sn 4+.
Embodiment 4
In embodiment 4, a kind of preparation of electroluminescent device, the embodiment 1 of usining makes light-emitting film as luminescent layer material; Wherein, the substrate of this electroluminescent device is glass, and anode layer is ITO (tin indium oxide), plays electric action, and both are combined, and are called ito glass, can buy acquisition.
1, select purity to be respectively 99.99% SrO, SrCl 2, P 2o 5, Ce 2o 3and SnO 2powder, according to mass percent: SrO～62.5%, SrCl 2～8%, Ce 2o 3～0.7%, SnO 2～1.8% and P 2o 5～27%, take SrO, SrCl 2, P 2o 5, Ce 2o 3and SnO 2the total mass number of powder is respectively 13.5g, 1.6g, 0.14g, 0.36g, 5.4g; After even mixing, sintering at 1250 ℃, naturally cooling, obtains target sample, and it is the target that 50mm, thickness are 2mm that target sample is cut into diameter;
2, target is packed in the vacuum cavity of magnetic-controlled sputtering coating equipment;
3, successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ito glass, and it is carried out to oxygen plasma treatment, put into the vacuum cavity of magnetic-controlled sputtering coating equipment after complete; Wherein, the base target spacing setting of target and ito glass is 60mm;
4, with mechanical pump and molecular pump, the vacuum tightness of the vacuum cavity of magnetic-controlled sputtering coating equipment is extracted into 5.0 * 10 -4pa;
5, adjust magnetron sputtering plating processing parameter: argon gas working gas flow is 25sccm; Magnetron sputtering operating pressure is 2.0Pa; Underlayer temperature is 500 ℃; Then be filmed the film sample obtaining, i.e. Sr 5(PO 4) 3cl:0.006Ce 3+, 0.018Sn 4+;
6, film sample is annealed in 0.01Pa vacuum oven 2h, annealing temperature is 700 ℃, obtains cerium tin codoped chlorine strontium phosphate light-emitting film;
7, adopt evaporation coating technique, the light-emitting film surface evaporation Ag layer in (6), as cathode layer, makes organic electroluminescence device.
Fig. 3 is electroluminescent spectrum (EL) figure that embodiment 4 obtains cerium tin codoped chlorine strontium phosphate light-emitting film.As shown in Figure 3, obtaining, in the electroluminescent spectrum (EL) of film, at 450nm and 480nm wavelength zone, having very strong glow peak, is the development material of electroluminescent device.
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 (8)

1. a cerium tin codoped chlorine strontium phosphate light-emitting film, is characterized in that, the chemical general formula of this light-emitting film is Sr 5(PO 4) 3cl x: mCe 3+, nSn 4+; Wherein, Sr 5(PO 4) 3cl xfor matrix, Ce 3+and Sn 4+for doped element; The span of x is that 0.8～1.2, m span is that 0.001～0.027, n span is 0.001～0.050.
2. cerium tin codoped chlorine strontium phosphate light-emitting film according to claim 1, is characterized in that, the value of x is that 1, m span is that 0.006, n span is 0.018.
3. a preparation method for cerium tin codoped chlorine strontium phosphate light-emitting film, is characterized in that, comprises the steps:
Step S1, according to chemical general formula Sr 5(PO 4) 3cl x: mCe 3+, nSn 4+in each element chemistry metering ratio, take SrO, SrCl 2, P 2o 5, CeO 2and SnO 2powder, after even mixing, sintering at 900～1300 ℃, makes target; Wherein, the span of x is that 0.8～1.2, m span is that 0.001～0.027, n span is 0.001～0.050;
Step S2, packs the target obtaining in step S1 and substrate in the vacuum cavity of magnetic-controlled sputtering coating equipment into, and the vacuum tightness of vacuum cavity is arranged on to 5 * 10 -4between Pa;
Step S3, adjustment magnetron sputtering plating processing parameter is: base target spacing is 45～90mm, magnetron sputtering operating pressure 0.2～4Pa, the flow 10～35sccm of argon gas working gas, underlayer temperature is 250 ℃～750 ℃; Then be filmed, obtain film sample;
Step S4,2h is processed in the film sample that step S3 is obtained vacuum annealing at 600 ℃, and obtaining chemical general formula is Sr 5(PO 4) 3cl x: mCe 3+, nSn 4+described cerium tin codoped chlorine strontium phosphate light-emitting film; Wherein, Sr 5(PO 4) 3cl xfor matrix, Ce 3+and Sn 4+for doped element.
4. the preparation method of cerium tin codoped chlorine strontium phosphate light-emitting film according to claim 3, is characterized in that, in described step S1, the value of x is that 1, m span is that 0.006, n span is 0.018.
5. according to the preparation method of the cerium tin codoped chlorine strontium phosphate light-emitting film described in claim 3 or 4, it is characterized in that, in described step S1, the sintering temperature of described preparation of target materials is 1250 ℃.
6. the Preparation Method of cerium tin codoped chlorine strontium phosphate light-emitting film processed according to claim 3, is characterized in that, in described step S3, described base target spacing is 60mm; Described magnetron sputtering operating pressure is 2.0Pa; The flow of described argon gas working gas is 25sccm; Described underlayer temperature is 500 ℃.
7. an organic electroluminescence device, this organic electroluminescence device is straticulate structure, this straticulate structure is followed successively by substrate, anode layer, luminescent layer and cathode layer, it is characterized in that, described luminescent layer is cerium tin codoped chlorine strontium phosphate light-emitting film, and the chemical general formula of this light-emitting film is Sr 5(PO 4) 3cl x: mCe 3+, nSn 4+; Wherein, Sr 5(PO 4) 3cl xfor matrix, Ce 3+and Sn 4+for doped element; The span of x is that 0.8～1.2, m span is that 0.001～0.027, n span is 0.001～0.050.
8. organic electroluminescence device according to claim 7, is characterized in that, the value of x is that 1, m span is that 0.006, n span is 0.018.
CN201110224340.9A 2011-08-05 2011-08-05 Cerium-tin-codoped strontium chlorophosphate light-emitting film and preparation method thereof, and organic electroluminescent device Active CN102911666B (en)

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Sr5(PO4)3Cl:Eu2+镧蓝色荧光粉合成新方法的研究;罗新宇等;《中国稀土学报》;20091031;第27卷(第5期);实验部分 *
罗新宇等.Sr5(PO4)3Cl:Eu2+镧蓝色荧光粉合成新方法的研究.《中国稀土学报》.2009,第27卷(第5期),实验部分. *

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