CN102838987A - Europium and cerium co-doped yttrium oxide luminescent film, preparation method thereof, and organic electroluminescent device - Google Patents

Europium and cerium co-doped yttrium oxide luminescent film, preparation method thereof, and organic electroluminescent device Download PDF

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CN102838987A
CN102838987A CN2011101700638A CN201110170063A CN102838987A CN 102838987 A CN102838987 A CN 102838987A CN 2011101700638 A CN2011101700638 A CN 2011101700638A CN 201110170063 A CN201110170063 A CN 201110170063A CN 102838987 A CN102838987 A CN 102838987A
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yttrium oxide
film
preparation
emitting film
europium
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CN102838987B (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 luminescent materials, and discloses a europium and cerium co-doped yttrium oxide luminescent film, a preparation method thereof, and an organic electroluminescent device. The luminescent film has a chemical general formula of Y2O3:xEu<+3>,yCe<+3>, wherein Y2O3 is a substrate, Ce<+3> and Eu<+3> are doped elements, x ranges from 0.0006 to 0.0327, and y ranges from 0.00007 to 0.007. According to the invention, a magnetron sputtering equipment is adopted for preparing the europium and cerium co-doped yttrium oxide luminescent film. The film has strong luminescence peak in 530nm and 610nm wavelength regions, and is a development material of electroluminescent devices.

Description

Europium cerium codoped yttrium oxide 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 europium cerium codoped yttrium oxide light-emitting film and preparation method thereof.The invention still further relates to a kind of organic electroluminescence device that uses this europium cerium codoped yttrium oxide light-emitting film as luminescent layer.
Background technology
Compare with the image display that traditional luminescent powder is made, light-emitting film contrast gradient, resolving power, thermal conduction, homogeneity, and aspects such as the tack of substrate, outgas speed all demonstrate stronger meliority.Therefore, as functional materials, light-emitting film has wide application prospect in such as cathode tube (CRTs), electroluminescent demonstration (ELDs) and FED FPD fields such as (FEDs).
In the research of LED fluorescent material, the emmission spectrum that rear-earth-doped yttrium oxide fluorescent luminescent powder, its excitation spectrum can mate existing near ultraviolet LED preferably can access good ruddiness exciting to blue light.But, be prepared into the film of electroluminescent device with europium cerium doped yttrium oxide class luminescent material, do not appear in the newspapers yet.
Summary of the invention
It is a kind of with Y that the object of the invention is to provide 2O 3For matrix, Ce and Eu element is the europium cerium codoped yttrium oxide light-emitting film of main luminescence center.
Europium cerium codoped yttrium oxide light-emitting film of the present invention, the chemical general formula of film is Y 2O 3: xEu + 3, yCe + 3Wherein, Y 2O 3Be matrix, Ce + 3And Eu + 3Be alloying element; The span of x is 0.0006～0.0327, and the span of y is 0.00007～0.007; The value of preferred x is 0.0049, and the value of y is 0.00056.
Another goal of the invention of the present invention is to provide the preparation method of above-mentioned europium cerium codoped yttrium oxide light-emitting film, and its preparation technology is following:
The preparation of step S1, ceramic target: according to chemical general formula Y 2O 3: xEu + 3, yCe + 3Each element chemistry metering ratio is selected Y for use 2O 3, Eu 2O 3And CeO 2Powder, through behind the uniform mixing, (preferred 1250 ℃ of following sintering obtain target at 900～1300 ℃; Wherein, the span of x is 0.0006～0.0327, and the span of y is 0.00007～0.007; Preferably, the value of x is 0.0049, and the value of y is 0.00056;
Step S2, with pack into the vacuum cavity of magnetron sputtering film device of the target among the step S1 and substrate, be evacuated to 1.0 * 10 to the vacuum tightness of cavity with mechanical pump and molecular pump -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 make film, 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 Y 2O 3: xEu + 3, yCe + 3Europium cerium codoped yttrium oxide light-emitting film; Wherein, Y 2O 3Be matrix, Ce + 3And Eu + 3Be alloying element.
The present invention also provides a kind of organic electroluminescence device, and this device is a 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 film is Y to europium cerium codoped yttrium oxide light-emitting film 2O 3: xEu + 3, yCe + 3Wherein, Y 2O 3Be matrix, Ce + 3And Eu + 3Be alloying element; The span of x is 0.0006～0.0327, and the span of y is 0.00007～0.007; Preferably, the value of x is 0.0049, and the value of y is 0.00056), substrate is a glass, and anode layer is ITO, and cathode layer is the Ag layer, and the Ag layer adopts evaporation process to be prepared in film surface.
The present invention adopts magnetron sputtering equipment, and preparation europium cerium codoped yttrium oxide light-emitting film obtains at 530nm and 610nm wavelength zone very strong glow peak being arranged all 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 europium cerium codoped yttrium oxide 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 europium cerium codoped yttrium oxide light-emitting film sample.
Embodiment
The present invention is in a kind of europium cerium codoped yttrium oxide light-emitting film that provides, and it is Y that this europium cerium codoped yttrium oxide light-emitting film comprises the film general formula 2O 3: xEu + 3, yCe + 3Wherein, Y 2O 3Be matrix, Ce + 3And Eu + 3Being alloying element, also is active element, and serves as main luminescence center; The span of x is 0.0006～0.0327, and the span of y is 0.00007～0.007; The value of preferred x is 0.0049, and the value of y is 0.00056.
Above-mentioned europium cerium codoped yttrium oxide light-emitting film preparation method provided by the invention, as shown in Figure 1, its preparation technology is following:
The preparation of step S1, ceramic target: according to chemical general formula Y 2O 3: xEu + 3, yCe + 3Each element chemistry metering ratio is selected Y for use 2O 3, Eu 2O 3And CeO 2Powder, through behind the uniform mixing, sintering under 900～1300 ℃ (preferred 1250 ℃), 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 0.0006～0.0327, and the span of y is 0.00007～0.007; The value of preferred x is 0.0049, and the value of y is 0.00056;
Step S2, with pack into the vacuum cavity of magnetron sputtering film device of the target among the step S1 and substrate, be evacuated to 1.0 * 10 to the vacuum tightness of cavity with mechanical pump and molecular pump -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 finishes, then make film, 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 Y 2O 3: xEu + 3, yCe + 3Said europium cerium codoped yttrium oxide light-emitting film; Wherein, Y 2O 3. be matrix, Ce + 3And Eu + 3Be alloying element.
Among the above-mentioned preparation method step S1, according to chemical general formula Y 2O 3: xEu + 3, yCe + 3Each element chemistry metering ratio, actual weighing Y 2O 3, CeO 2And Eu 2O 3During powder, by mass percentage: CeO 2Account for 0.01～1wt% of total amount, preferred 0.08wt%; Eu 2O 3Account for 0.01～5wt% of total amount, preferred 0.75wt%; Y 2O 3Account for 94～99.98wt% of total amount, preferred 99.17wt%.
The present invention also provides a kind of organic electroluminescence device, and is as shown in Figure 2, and this device is a 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 a glass, and anode layer is the ITO layer, and promptly ito glass can be bought acquisition; (chemical general formula of this film is Y to luminescent layer 3 for europium cerium codoped yttrium oxide light-emitting film layer 2O 3: xEu + 3, yCe + 3Wherein, Y 2O 3Be matrix, Ce and Eu are alloying element; The span of x is 0.0006～0.0327, and the span of y is 0.00007～0.007; Preferably, the value of x is 0.0049, and the value of y is 0.00056); Cathode layer 4 is the Ag layer, and the Ag layer adopts evaporation process to be prepared in film surface.
Below in conjunction with accompanying drawing, further explain is done in preferred embodiment of the present invention.
Embodiment 1
1, select for use purity to be respectively 99.99% Y 2O 3, CeO 2And Eu 2O 3Powder (wherein, Y 2O 3Quality be 198.34g, CeO 2Quality be 0.16g, Eu 2O 3Quality be 1.5g), through behind the uniform mixing, at 1250 ℃ of following sintering, naturally cooling obtains the target sample, 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 magnetron sputtering film device;
3, carry out oxygen plasma treatment successively with acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass, and to it, put into the vacuum cavity of magnetron sputtering film device after finishing; Wherein, the basic target spacing of target and glass is set at 60mm;
4, be extracted into 5.0 * 10 to the vacuum tightness of the vacuum cavity of magnetron sputtering film device with mechanical pump and molecular pump -4Pa;
5, adjustment 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 make film, the film sample that obtains;
6, with the film sample 2h that in the 0.01Pa vacuum oven, anneals, annealing temperature is 600 ℃, obtains europium cerium codoped yttrium oxide light-emitting film, i.e. Y 2O 3: 0.0049Eu + 3, 0.00056Ce + 3
Embodiment 2
1,, select for use purity to be respectively 99.99% Y 2O 3, CeO 2And Eu 2O 3Powder (wherein, Y 2O 3Quality be 199.96g, CeO 2Quality be 0.002g, Eu 2O 3Quality be 0.002g), through behind the uniform mixing, at 900 ℃ of following sintering, naturally cooling obtains the target sample, 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 magnetron sputtering film device;
3, carry out oxygen plasma treatment successively with acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass, and to it, put into the vacuum cavity of magnetron sputtering film device after finishing; Wherein, the basic target spacing of target and glass is set at 45mm;
4, be extracted into 1.0 * 10 to the vacuum tightness of the vacuum cavity of magnetron sputtering film device with mechanical pump and molecular pump -3Pa;
5, adjustment magnetron sputtering plating processing parameter: argon gas working gas flow is 10sccm; The magnetron sputtering operating pressure is 4Pa; Underlayer temperature is 250 ℃; Then make film, the film sample that obtains;
6, with the film sample 1h that in the 0.01Pa vacuum oven, anneals, annealing temperature is 500 ℃, obtains europium cerium codoped yttrium oxide light-emitting film, i.e. Y 2O 3: 0.0006Eu + 3, 0.00007Ce + 3
Embodiment 3
1, select for use purity to be respectively 99.99% Y 2O 3, CeO 2And Eu 2O 3Powder (wherein, Y 2O 3Quality be 188g, CeO 2Quality be 6g, Eu 2O 3Quality be 10g), through behind the uniform mixing, at 1300 ℃ of following sintering, naturally cooling obtains the target sample, 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 magnetron sputtering film device;
3, carry out oxygen plasma treatment successively with acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning band glass substrate, and to it, put into the vacuum cavity of magnetron sputtering film device after finishing; Wherein, the basic target spacing of target and glass is set at 90mm;
4, be extracted into 1.0 * 10 to the vacuum tightness of the vacuum cavity of magnetron sputtering film device with mechanical pump and molecular pump -5Pa;
5, adjustment 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 make film, the film sample that obtains;
6, with the film sample 3h that in the 0.01Pa vacuum oven, anneals, annealing temperature is 800 ℃, obtains europium cerium codoped yttrium oxide light-emitting film, i.e. Y 2O 3: 0.0327Eu + 3, 0.007Ce + 3
Among the following embodiment 4, substrate is a glass, and anode layer is ITO, plays electric action, and both lump together, and are called ito glass, can buy acquisition.
Embodiment 4
1, select for use purity to be respectively 99.99% Y 2O 3, CeO 2And Eu 2O 3Powder (wherein, Y 2O 3Quality be 193.8g, CeO 2Quality be 6g, Eu 2O 3Quality be 0.02g), through behind the uniform mixing, at 1250 ℃ of following sintering, naturally cooling obtains the target sample, 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 magnetron sputtering film device;
3, carry out oxygen plasma treatment successively with acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning band ito glass, and to it, put into the vacuum cavity of magnetron sputtering film device after finishing; Wherein, the basic target spacing of target and ito glass is set at 60mm;
4, be extracted into 5.0 * 10 to the vacuum tightness of the vacuum cavity of magnetron sputtering film device with mechanical pump and molecular pump -4Pa;
5, adjustment 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 make film, the film sample that obtains, i.e. Y 2O 3: 0.0006Eu + 3, 0.007Ce + 3
6, with the film sample 2h that in the 0.01Pa vacuum oven, anneals, annealing temperature is 700 ℃, obtains europium cerium codoped yttrium oxide light-emitting film;
7, adopt evaporation coating technique, the light-emitting film surface vapor deposition Ag layer in (6) as cathode layer, makes organic electroluminescence device.
Fig. 3 is electroluminescent spectrum (EL) figure that embodiment 4 obtains europium cerium codoped yttrium oxide light-emitting film sample.Can be known by Fig. 3, obtain at 530nm and 610nm wavelength zone very strong glow peak being arranged all in the electroluminescent spectrum (EL) of film, be the development material of electroluminescent device.
Should be understood that above-mentioned statement to 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 accompanying claims.

Claims (10)

1. an europium cerium codoped yttrium oxide light-emitting film is characterized in that the chemical general formula of this light-emitting film is Y 2O 3: xEu + 3, yCe + 3Wherein, Y 2O 3Be matrix, Ce + 3And Eu + 3Be alloying element; The span of x is 0.0006～0.0327, and the span of y is 0.00007～0.007.
2. europium cerium codoped yttrium oxide light-emitting film according to claim 1 is characterized in that the value of x is 0.0049, and the value of y is 0.00056.
3. the preparation method of an europium cerium codoped yttrium oxide light-emitting film is characterized in that, comprises the steps:
Step S1 is according to chemical general formula Y 2O 3: xEu + 3, yCe + 3Each element chemistry metering ratio takes by weighing Y 2O 3, Eu 2O 3And CeO 2Powder through behind the uniform mixing, at 900～1300 ℃ of following sintering, is processed target; Wherein, the span of x is 0.0006～0.0327, and the span of y is 0.00007～0.007;
Step S2 with pack into the vacuum cavity of magnetron sputtering film device of the target that obtains among the step S1 and substrate, and is arranged on 1.0 * 10 with the vacuum tightness of vacuum cavity -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 make film, obtain film sample;
Step S4 handles 1～3h with the film sample that step S3 obtains in 500～800 ℃ of following vacuum annealings, and obtaining chemical general formula is Y 2O 3: xEu + 3, yCe + 3Said europium cerium codoped yttrium oxide light-emitting film; Wherein, Y 2O 3Be matrix, Ce + 3And Eu + 3Be alloying element.
4. the preparation method of europium cerium codoped yttrium oxide light-emitting film according to claim 3 is characterized in that among the said step S1, the span of x is 0.0049, and the span of y is 0.00056.
5. according to the preparation method of claim 3 or 4 described europium cerium codoped yttrium oxide light-emitting films, it is characterized in that among the said step S1, the sintering temperature of said target preparation is 1250 ℃.
6. the preparation method of europium cerium codoped yttrium oxide light-emitting film according to claim 3 is characterized in that among the said step S2, the vacuum tightness of vacuum cavity is arranged on 5.0 * 10 -4Pa.
7. the Preparation Method of system europium cerium codoped yttrium oxide light-emitting film according to claim 3 is characterized in that among the said step S3, said basic target spacing is 60mm; Said magnetron sputtering operating pressure is 2.0Pa; The flow of said argon gas working gas is 25sccm; Said underlayer temperature is 500 ℃.
8. the preparation method of europium cerium codoped yttrium oxide light-emitting film according to claim 3 is characterized in that among the said step S4, the annealing temperature in the said anneal process is 600 ℃, and annealing time is 2h.
9. organic electroluminescence device; This organic electroluminescence device is a straticulate structure, and this straticulate structure is followed successively by substrate, anode layer, luminescent layer and cathode layer, it is characterized in that; Said luminescent layer is an europium cerium codoped yttrium oxide light-emitting film, and the chemical general formula of this light-emitting film is Y 2O 3: xEu + 3, yCe + 3Wherein, the span of x is 0.0006～0.0327, and the span of y is 0.00007～0.007.
10. organic electroluminescence device according to claim 9 is characterized in that, the value of x is 0.0049, and the value of y is 0.00056.
CN201110170063.8A 2011-06-22 2011-06-22 Europium and cerium co-doped yttrium oxide luminescent film, preparation method thereof, and organic electroluminescent device Active CN102838987B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113488596A (en) * 2021-06-30 2021-10-08 华中科技大学 Ce3+Halogenide electroluminescent device

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Publication number Priority date Publication date Assignee Title
JPS55110181A (en) * 1979-02-20 1980-08-25 Futaba Corp Fluorescent material
US5367172A (en) * 1993-06-01 1994-11-22 E. I. Du Pont De Nemours And Company Radiological system employing phosphors of different densities
CN1523077A (en) * 2003-09-05 2004-08-25 �й���ѧԺ�����о��� Method for preparing rare earth oxide group nanometer luminescent powder

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS55110181A (en) * 1979-02-20 1980-08-25 Futaba Corp Fluorescent material
US5367172A (en) * 1993-06-01 1994-11-22 E. I. Du Pont De Nemours And Company Radiological system employing phosphors of different densities
CN1523077A (en) * 2003-09-05 2004-08-25 �й���ѧԺ�����о��� Method for preparing rare earth oxide group nanometer luminescent powder

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113488596A (en) * 2021-06-30 2021-10-08 华中科技大学 Ce3+Halogenide electroluminescent device
CN113488596B (en) * 2021-06-30 2022-05-20 华中科技大学 Ce3+Electroluminescent device based on halides

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