CN102911666A - 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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CN102911666A
CN102911666A CN2011102243409A CN201110224340A CN102911666A CN 102911666 A CN102911666 A CN 102911666A CN 2011102243409 A CN2011102243409 A CN 2011102243409A CN 201110224340 A CN201110224340 A CN 201110224340A CN 102911666 A CN102911666 A CN 102911666A
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CN102911666B (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 aspects 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 is widely used in the electroluminescent device production as the red-green glow fluorescent material.But, be prepared into electroluminescent film with alkaline-earth metal halide phosphate class luminescent material, still rarely seen report.
Summary of the invention
The object of the invention be to provide a kind of take the chlorine strontium phosphate as matrix, cerium and tin element be the cerium tin codoped chlorine strontium phosphate light-emitting film of main luminescence center.
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 xBe matrix, Ce 3+And Sn 4+Be 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; The value of preferred 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 evenly mixing, at 900～1300 ℃ (preferred 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; The value of preferred x is that 1, m span is that 0.006, n span is 0.018.
Step S2, with pack into the vacuum cavity of magnetic-controlled sputtering coating equipment of the target among the step S1 and substrate, with mechanical pump and molecular pump the vacuum tightness of cavity is evacuated to 1.0 * 10 -3Pa～1.0 * 10 -5Pa, preferred vacuum tightness is 5.0 * 10 -4Pa;
Step S3, adjustment magnetron sputtering plating processing parameter are: basic target spacing is 45～90mm, preferred 60mm; Underlayer temperature is 250 ℃～750 ℃, preferred 500 ℃; Gas flow 10～the 35sccm of argon gas working gas, preferred 25sccm; Magnetron sputtering operating pressure 0.2～4Pa, preferred 2.0Pa; After processing parameter has been adjusted, then be filmed, obtain film sample;
Step S4, the film sample that step S3 is obtained place vacuum oven, (being 0.01Pa) anneal 1～3h under 500～800 ℃ (preferred 600 ℃), vacuum state (preferred 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 xBe matrix, Ce 3+And Sn 4+Be 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 xBe matrix, Ce 3+And Sn 4+Be 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; The value of preferred 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 the Ag layer, and the Ag layer adopts the evaporation process preparation at film surface.
The present invention adopts magnetron sputtering equipment, and preparation cerium tin codoped chlorine strontium phosphate light-emitting film obtains at 450nm and 480nm wavelength zone very strong glow peak being arranged in the electroluminescent spectrum (EL) of film, is the development material of electroluminescent device.
Description of drawings
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 the film general formula 5(PO 4) 3Cl x: mCe 3+, nSn 4+Wherein, Sr 5(PO 4) 3Cl xBe matrix, Ce 3+And Sn 4+Being doped element, also is active element, and serves 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 of preferred x is that the value of 1, m is that the value of 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 evenly mixing, at 900～1300 ℃ (preferred 1250 ℃) lower sintering, naturally cooling obtains the target sample, and it is that 50mm, thickness are the target of 2mm that the 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 the value of preferred x is that 1, m span is that 0.006, n span is 0.018;
Step S2, with pack into the vacuum cavity of magnetic-controlled sputtering coating equipment of the target among the step S1 and substrate, with mechanical pump and molecular pump the vacuum tightness of cavity is evacuated to 1.0 * 10 -3Pa～1.0 * 10 -5Pa, preferred 5.0 * 10 -4Pa;
Step S3, adjustment magnetron sputtering plating processing parameter are: basic target spacing is 45～90mm, preferred 60mm; Underlayer temperature is 250 ℃～750 ℃, preferred 500 ℃; Gas flow 10～the 35sccm of argon gas working gas, preferred 25sccm; Magnetron sputtering operating pressure 0.2～4Pa, preferred 2.0Pa; After the processing parameter adjustment is complete, then be filmed, obtain film sample;
Step S4, the film sample that step S3 is obtained place vacuum oven, (being 0.01Pa) anneal 1～3h under 500～800 ℃ (preferred 600 ℃), vacuum state (preferred 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 xBe matrix, Ce 3+And Sn 4+Be doped element.
Among the 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, the n span is 0.001～0.050, and the value of preferred x is that 1, m span is 0.006, the n span is 0.018) in each element chemistry metering ratio, actual weighing SrO, SrCl 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 the ITO layer, and namely ito glass can be bought acquisition; (chemical general formula of this light-emitting film is Sr to luminescent layer 3 for cerium tin codoped chlorine strontium phosphate light-emitting film layer 5(PO 4) 3Cl x: mCe 3+, nSn 4+Wherein, Sr 5(PO 4) 3Cl xBe matrix, Ce 3+And Sn 4+Be doped element; The span of x is 0.8～1.2, the m span is 0.001～0.027, the n span is 0.001～0.050, the value of preferred 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 the Ag layer, and the Ag layer adopts the evaporation process preparation at film surface.
The present invention adopts magnetron sputtering equipment, and preparation cerium tin codoped chlorine strontium phosphate light-emitting film obtains at 450nm and 480nm wavelength zone very strong glow peak being arranged in the electroluminescent spectrum (EL) of film, 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 is 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 by weighing 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 are through after evenly mixing, and at 1250 ℃ of lower sintering, naturally cooling obtains the target sample, and it is that 50mm, thickness are the target of 2mm that the target sample is cut into diameter;
2, target is packed in the vacuum cavity of magnetic-controlled sputtering coating equipment;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass, and to it, put into the vacuum cavity of magnetic-controlled sputtering coating equipment after complete; Wherein, the basic 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 the magnetron sputtering plating processing parameter: argon gas working gas flow is 25sccm; The magnetron sputtering operating pressure is 2.0Pa; Underlayer temperature is 500 ℃; Then be filmed the film sample that obtains;
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 is according to mass percent: SrO～56.9%, SrCl 2～15%, Ce 2O 3～0.1%, SnO 2～5% and P 2O 5～23%, take by weighing 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 are through after evenly mixing, and at 900 ℃ of lower sintering, naturally cooling obtains the target sample, and it is that 50mm, thickness are the target of 2mm that the target sample is cut into diameter;
2, target is packed in the vacuum cavity of magnetic-controlled sputtering coating equipment;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass, and to it, put into the vacuum cavity of magnetic-controlled sputtering coating equipment after complete; Wherein, the basic 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 the magnetron sputtering plating processing parameter: argon gas working gas flow is 10sccm; The magnetron sputtering operating pressure is 4Pa; Underlayer temperature is 250 ℃; Then be filmed the film sample that obtains;
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 is according to mass percent: SrO～70%, SrCl 2～5%, Ce 2O 3～3% He, SnO 2～0.1%, P 2O 5～21.9%, take by weighing 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 are through after evenly mixing, and at 1300 ℃ of lower sintering, naturally cooling obtains the target sample, and it is that 50mm, thickness are the target of 2mm that the target sample is cut into diameter;
2, target is packed in the vacuum cavity of magnetic-controlled sputtering coating equipment;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning band glass substrate, and to it, put into the vacuum cavity of magnetic-controlled sputtering coating equipment after complete; Wherein, the basic 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 the magnetron sputtering plating processing parameter: argon gas working gas flow is 35sccm; The magnetron sputtering operating pressure is 0.2Pa; Underlayer temperature is 750 ℃; Then be filmed the film sample that obtains;
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
Among the embodiment 4, a kind of preparation of electroluminescent device makes light-emitting film as the luminescent layer material with embodiment 1; 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 is 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 by weighing 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 evenly mixing, at 1250 ℃ of lower sintering, naturally cooling obtains the target sample, and it is that 50mm, thickness are the target of 2mm that the target sample is cut into diameter;
2, target is packed in the vacuum cavity of magnetic-controlled sputtering coating equipment;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ito glass, and to it, put into the vacuum cavity of magnetic-controlled sputtering coating equipment after complete; Wherein, the basic 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 the magnetron sputtering plating processing parameter: argon gas working gas flow is 25sccm; The magnetron sputtering operating pressure is 2.0Pa; Underlayer temperature is 500 ℃; Then be filmed the film sample that obtains, 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 at 450nm and 480nm wavelength zone very strong glow peak being arranged in the electroluminescent spectrum (EL) of film, is the development material of electroluminescent device.
Should be understood that 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, scope of patent protection of the present invention should be as the criterion with claims.

Claims (10)

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 xBe matrix, Ce 3+And Sn 4+Be 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. the preparation method of a cerium tin codoped chlorine strontium phosphate light-emitting film is characterized in that, comprises the steps:
Step S1 is according to chemical general formula Sr 5(PO 4) 3Cl x: mCe 3+, nSn 4+In each element chemistry metering ratio, take by weighing SrO, SrCl 2, P 2O 5, CeO 2And SnO 2Powder after evenly mixing, at 900～1300 ℃ of lower sintering, is made 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 that obtains among the 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 1.0 * 10 -3Pa～1.0 * 10 -5Between the Pa;
Step S3, adjustment magnetron sputtering plating processing parameter is: basic target spacing is 45～90mm, and magnetron sputtering operating pressure 0.2～4Pa, the flow 10～35sccm of argon gas working gas, underlayer temperature are 250 ℃～750 ℃; Then be filmed, obtain film sample;
Step S4 processes 1～3h with the film sample that step S3 obtains in 500～800 ℃ of lower vacuum annealings, 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 xBe matrix, Ce 3+And Sn 4+Be doped element.
4. the preparation method of cerium tin codoped chlorine strontium phosphate light-emitting film according to claim 3 is characterized in that, among the described step S1, the value of x is that 1, m span is that 0.006, n span is 0.018.
5. according to claim 3 or the preparation method of 4 described cerium tin codoped chlorine strontium phosphate light-emitting films, it is characterized in that among the 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 according to claim 3 is characterized in that among the described step S2, the vacuum tightness of described vacuum cavity is arranged on 5.0 * 10 -4Pa.
7. the Preparation Method of cerium tin codoped chlorine strontium phosphate light-emitting film processed according to claim 3 is characterized in that, among the described step S3, described basic 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 ℃.
8. the preparation method of cerium tin codoped chlorine strontium phosphate light-emitting film according to claim 3 is characterized in that, among the described step S4, the annealing temperature during described vacuum annealing is processed is 600 ℃, and annealing time is 2h.
9. 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 xBe matrix, Ce 3+And Sn 4+Be 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.
10. organic electroluminescence device according to claim 9 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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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104178154A (en) * 2013-05-23 2014-12-03 海洋王照明科技股份有限公司 Samarium-doped fluorine beryllium phosphate light-emitting film and preparation method thereof and electroluminescent device

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
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》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104178154A (en) * 2013-05-23 2014-12-03 海洋王照明科技股份有限公司 Samarium-doped fluorine beryllium phosphate light-emitting film and preparation method thereof and electroluminescent device

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