CN104650860A - Cerium-doped three-family silicon nitride luminescence film, preparation method and application thereof - Google Patents

Cerium-doped three-family silicon nitride luminescence film, preparation method and application thereof Download PDF

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CN104650860A
CN104650860A CN201310578442.XA CN201310578442A CN104650860A CN 104650860 A CN104650860 A CN 104650860A CN 201310578442 A CN201310578442 A CN 201310578442A CN 104650860 A CN104650860 A CN 104650860A
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cerium
group iii
iii nitride
emitting film
nitride silicon
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周明杰
陈吉星
王平
钟铁涛
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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 relates to a cerium-doped three-family silicon nitride luminescence film, which has a chemical formula of Me2Si6N10: xCe<3+>, wherein, x is greater than or equal to 0.01, and x is less than or equal to 0.05, Me2Si6N10 is a matrix, cerium element is an activation element, Me is at least one of Al, Ga, In and T1. In a photoluminescence spectrum of the cerium-doped three-family silicon nitride luminescence film, strong luminescence peaks of the cerium-doped three-family silicon nitride luminescence film are generated at 620nm, the cerium-doped three-family silicon nitride luminescence film can be used in a thin-film electroluminescence display, and the invention also provides a preparation method and an application of the cerium-doped three-family silicon nitride luminescence film.

Description

Cerium dopping Group III nitride silicon light-emitting film, preparation method and application thereof
[technical field]
The present invention relates to a kind of cerium dopping Group III nitride silicon light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof.
[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 film of exploitation multiband luminescence is the developing direction of this problem.But, can be applicable to the cerium dopping Group III nitride silicon light-emitting film of thin-film electroluminescent displays, have not yet to see report.
[summary of the invention]
Based on this, be necessary to provide a kind of the cerium dopping Group III nitride silicon light-emitting film, this cerium dopping Group III nitride silicon light-emitting film electroluminescent device of its preparation method and preparation method thereof that can be applicable to membrane electro luminescent device.
A kind of cerium dopping Group III nitride silicon light-emitting film, its chemical formula is Me 2si 6n 10: xCe 3+, wherein, 0.01≤x≤0.05, Me 2si 6n 10be matrix, Ce elements is active element, and Me is at least one in Al, Ga, In and Tl.
The thickness of described cerium dopping Group III nitride silicon light-emitting film is 80nm ~ 300nm.
A preparation method for cerium dopping Group III nitride silicon light-emitting film, comprises the following steps:
Substrate is loaded in the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10 -2pa ~ 1.0 × 10 -3pa;
Regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, adopts the carrier of argon stream, according to Me 2si 6n 10: xCe 3+the stoichiometric ratio of each element is by (DPM) 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium pass in reaction chamber, and
Then pass into ammonia, carrying out chemical vapour deposition, to obtain its chemical formula of cerium dopping Group III nitride silicon light-emitting film be Me 2si 6n 10: xCe 3+cerium dopping Group III nitride silicon light-emitting film, wherein, 0.01≤x≤0.05, Me 2si 6n 10be matrix, Ce elements is active element, and Me is at least one in Al, Ga, In and Tl.
Described (DPM) 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium mol ratio are 2:6:(0.01 ~ 0.05);
Described (DPM) 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium mol ratio are 2:6:0.03;
Described argon stream amount is 5 ~ 15sccm, and ammonia airshed is 10 ~ 200sccm.
A kind of membrane electro luminescent device, this membrane electro luminescent device comprises the substrate, anode layer, luminescent layer and the cathode layer that stack gradually, the material of described luminescent layer is cerium dopping Group III nitride silicon light-emitting film, and the chemical formula of this cerium dopping Group III nitride silicon light-emitting film is Me 2si 6n 10: xCe 3+, wherein, 0.01≤x≤0.05, Me 2si 6n 10be matrix, Ce elements is active element, and Me is at least one in Al, Ga, In and Tl.
A preparation method for membrane electro luminescent device, comprises the following steps:
The substrate with anode is provided;
Described anode forms luminescent layer, and the material of described luminescent layer is cerium dopping Group III nitride silicon light-emitting film, and the chemical formula of this cerium dopping Group III nitride silicon light-emitting film is Me 2si 6n 10: xCe 3+, wherein, 0.01≤x≤0.05, Me 2si 6n 10be matrix, Ce elements is active element, and Me is at least one in Al, Ga, In and Tl;
Form negative electrode on the light-emitting layer.
In a preferred embodiment, the preparation of described luminescent layer comprises the following steps:
Substrate is loaded in the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10 -2pa ~ 1.0 × 10 -3pa;
Regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, adopts the carrier of argon stream, according to Me 2si 6n 10: xCe 3+the stoichiometric ratio of each element is by (DPM) 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium pass in reaction chamber, and wherein, argon stream amount is 5 ~ 15sccm, and
Then pass into ammonia, flow is 10 ~ 200sccm; Carrying out chemical vapour deposition, to obtain luminescent layer chemical formula be Me 2si 6n 10: xCe 3+, wherein, 0.01≤x≤0.05, Me 2si 6n 10be matrix, Ce elements is active element, and Me is at least one in Al, Ga, In and Tl.
Above-mentioned cerium dopping Group III nitride silicon light-emitting film (Me 2si 6n 10: xCe 3+) electroluminescent spectrum (EL) in, have very strong glow peak in 620nm wavelength zone, can be applied in thin-film electroluminescent displays.
[accompanying drawing explanation]
Fig. 1 is the structural representation of the membrane electro luminescent device of an embodiment;
Fig. 2 is the electroluminescent spectrogram of cerium dopping Group III nitride silicon light-emitting film prepared by embodiment 1;
Fig. 3 is the XRD figure of cerium dopping Group III nitride silicon light-emitting film prepared by embodiment 1;
Fig. 4 is the voltage of membrane electro luminescent device prepared of embodiment 1 and electric current and brightness relationship figure.
[embodiment]
Below in conjunction with the drawings and specific embodiments, cerium dopping Group III nitride silicon light-emitting film, its preparation method and membrane electro luminescent device and preparation method thereof are illustrated further.
The cerium dopping Group III nitride silicon light-emitting film of one embodiment, its chemical formula is Me 2si 6n 10: xCe 3+, wherein, 0.01≤x≤0.05, Me 2si 6n 10be matrix, Ce elements is active element, and Me is at least one in Al, Ga, In and Tl.
Preferably, the thickness of cerium dopping Group III nitride silicon light-emitting film is 80nm ~ 300nm, x is 0.03.
Me in this cerium dopping Group III nitride silicon light-emitting film 2si 6n 10be matrix, Ce elements is active element.In the electroluminescent spectrum (EL) of this cerium dopping Group III nitride silicon light-emitting film, there is very strong glow peak in 620nm wavelength zone, can be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned cerium dopping Group III nitride silicon light-emitting film, comprises the following steps:
Step S11, substrate to be loaded in the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10 -2p a~ 1.0 × 10 -3p a.
In the present embodiment, substrate is indium tin oxide glass (ITO), is appreciated that in other embodiments, can be also fluorine doped tin oxide glass (FTO), mixes the zinc oxide (AZO) of aluminium or mix the zinc oxide (IZO) of indium; Substrate priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, the air-dry rear feeding reaction chamber of nitrogen;
Preferably, the vacuum tightness of reaction chamber is 4.0 × 10 -3pa.
Step S12, by substrate thermal treatment 10 minutes ~ 30 minutes at 600 DEG C ~ 800 DEG C.
Step S13, adjustment substrate temperature are 250 DEG C ~ 650 DEG C, and rotating speed is 50 revs/min ~ 1000 revs/min, adopts the carrier of argon stream, according to Me 2si 6n 10: xCe 3+the stoichiometric ratio of each element is by (DPM) 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium pass in reaction chamber;
In a preferred embodiment, (DPM) 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium mol ratio are 2:6:(0.01 ~ 0.05);
In a more preferred embodiment, (DPM) 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium mol ratio are 2:6:0.03,
In a preferred embodiment, substrate temperature is preferably 500 DEG C, and the rotating speed of substrate is preferably 300 revs/min, and argon stream amount is 5 ~ 15sccm;
In more preferred embodiment, argon stream amount is 10sccm;
Step S14, then pass into ammonia, carrying out chemical vapour deposition, to obtain its chemical formula of cerium dopping Group III nitride silicon light-emitting film be Me 2si 6n 10: xCe 3+, wherein, 0.01≤x≤0.05, Me 2si 6n 10be matrix, Ce elements is active element, and Me is at least one in Al, Ga, In and Tl.
In a preferred embodiment, ammonia airshed is 10 ~ 200sccm, x is 0.03.
In more preferred embodiment, ammonia airshed is 120sccm.
Stop passing into (DPM) after step S15, deposition 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium and argon gas, continue to pass into ammonia and make the temperature of cerium dopping Group III nitride silicon light-emitting film be down to 80 DEG C ~ 150 DEG C.
In present embodiment, preferably, the temperature of cerium dopping Group III nitride silicon light-emitting film is made to be down to 100 DEG C.
Be appreciated that step S12 and step S15 can omit.
Refer to Fig. 1, the membrane electro luminescent device of an embodiment, this membrane electro luminescent device comprises the substrate 1, anode 2, luminescent layer 3 and the negative electrode 4 that stack gradually.
Substrate 1 is glass substrate.Anode 2 is for being formed at the tin indium oxide (ITO) in glass substrate.The material of luminescent layer 3 is cerium dopping Group III nitride silicon light-emitting film, and the chemical formula of this cerium dopping Group III nitride silicon light-emitting film is Me 2si 6n 10: xCe 3+, wherein, 0.01≤x≤0.05, Me 2si 6n 10be matrix, Ce elements is active element, and Me is at least one in Al, Ga, In and Tl.The material of negative electrode 4 is silver (Ag).
The preparation method of above-mentioned membrane electro luminescent device, comprises the following steps:
Step S21, provide the substrate 1 with anode 2.
In present embodiment, substrate 1 is glass substrate, and anode 2 is for being formed at the tin indium oxide (ITO) in glass substrate.Be appreciated that in other embodiments, can be also fluorine doped tin oxide glass (FTO), mix the zinc oxide (AZO) of aluminium or mix the zinc oxide (IZO) of indium; There is the substrate 1 priority acetone of anode 2, dehydrated alcohol and deionized water ultrasonic cleaning and carry out oxygen plasma treatment with to it.
Step S22, on anode 2, form luminescent layer 3, the material of luminescent layer 3 is cerium dopping Group III nitride silicon light-emitting film, and the chemical formula of this cerium dopping Group III nitride silicon light-emitting film is Me 2si 6n 10: xCe 3+, wherein, 0.01≤x≤0.05, Me 2si 6n 10be matrix, Ce elements is active element, and Me is at least one in Al, Ga, In and Tl.
In present embodiment, luminescent layer 3 is obtained by following steps:
First, substrate is loaded in the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10 -2pa ~ 1.0 × 10 -3pa;
Moreover, by substrate thermal treatment 10 minutes ~ 30 minutes at 600 DEG C ~ 800 DEG C.Also can without the need to this step.
Secondly, regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, adopts the carrier of argon stream, according to Me 2si 6n 10: xCe 3+the stoichiometric ratio of each element is by (DPM) 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium pass in reaction chamber;
In a preferred embodiment, (DPM) 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium mol ratio are 2:6:(0.01 ~ 0.05);
In a more preferred embodiment, (DPM) 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium mol ratio are 2:6:0.03;
In a preferred embodiment, substrate temperature is preferably 500 DEG C, and the rotating speed of substrate is preferably 300 revs/min, and argon stream amount is 5 ~ 15sccm;
In more preferred embodiment, argon stream amount is 10sccm;
Then pass into ammonia, carry out chemical vapour deposition film and form luminescent layer on described anode.
In preferred embodiment, the flow of ammonia is preferably 10 ~ 200sccm;
In more preferred embodiment, ammonia airshed is 120sccm.
Finally, stop passing into (DPM) after deposition 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium and argon gas, continue to pass into ammonia and make the temperature of cerium dopping Group III nitride silicon light-emitting film be down to 80 DEG C ~ 150 DEG C.
In present embodiment, preferably, the temperature of cerium dopping Group III nitride silicon light-emitting film is made to be down to 100 DEG C.Can without the need to this step.
Step S23, on luminescent layer 3, form negative electrode 4.
In present embodiment, the material of negative electrode 4 is silver (Ag), is formed by evaporation.
Be specific embodiment below.
Embodiment 1
Substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 4.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, passes into organic source (DPM) 3the mol ratio of Al, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium is 2:6:0.03, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into ammonia, ammonia airshed is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, and continue logical ammonia, temperature drops to less than 100 DEG C, takes out sample Al 2si 6n 10: 0.03Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula of the cerium dopping Group III nitride silicon light-emitting film obtained in the present embodiment is Al 2si 6n 10: 0.03Ce 3+, wherein Al 2si 6n 10be matrix, Ce elements is active element.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the cerium dopping Group III nitride silicon light-emitting film that embodiment 1 obtains.As seen from Figure 2, the electroluminescent spectral curve of cerium dopping Group III nitride silicon light-emitting film that embodiment 1 obtains has very strong glow peak can be applied in thin-film electroluminescent displays in 620nm wavelength zone.
Refer to Fig. 3, Fig. 3 is the XRD curve of cerium dopping Group III nitride silicon light-emitting film prepared by embodiment 1, test comparison standard P DF card.As can be seen from Figure 3 the diffraction peak shown in figure is the peak crystallization of Group III nitride silicon, does not occur the diffraction peak of doped element and other impurity; Illustrate that the product that this preparation method obtains has good crystalline quality.
Refer to Fig. 4, Fig. 4 is the voltage of membrane electro luminescent device prepared of embodiment 1 and electric current and brightness relationship figure, curve 1 is voltage and current density relation curve in figure 4, device luminescence from voltage 5.5V can be found out, curve 2 is voltage and brightness relationship curve, can find out that the high-high brightness of this device is 160cd/m 2, show that device has the good characteristics of luminescence.
Embodiment 2
Substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, passes into organic source (DPM) 3the mol ratio of Al, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium is 2:6:0.06, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into ammonia, ammonia airshed is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, and continue logical ammonia, temperature drops to less than 100 DEG C, takes out sample Al 2si 6n 10: 0.06Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 3
Substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, passes into organic source (DPM) 3the mol ratio of Al, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium is 2:6:0.01, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into ammonia, ammonia airshed is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, and continue logical ammonia, temperature drops to less than 100 DEG C, takes out sample Al 2si 6n 10: 0.01Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 4: substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 4.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, passes into organic source (DPM) 3the mol ratio of Ga, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium is 2:6:0.03, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into ammonia, ammonia airshed is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, and continue logical ammonia, temperature drops to less than 100 DEG C, takes out sample Ga 2si 6n 10: 0.03Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 5: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, passes into organic source (DPM) 3the mol ratio of Ga, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium is 2:6:0.06, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into ammonia, ammonia airshed is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, and continue logical ammonia, temperature drops to less than 100 DEG C, takes out sample Ga 2si 6n 10: 0.06Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 6: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, passes into organic source (DPM) 3the mol ratio of Ga, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium is 2:6:0.01, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into ammonia, ammonia airshed is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, and continue logical ammonia, temperature drops to less than 100 DEG C, takes out sample Ga 2si 6n 10: 0.01Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 7: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 4.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, passes into organic source (DPM) 3the mol ratio of In, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium is 2:6:0.03, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into ammonia, ammonia airshed is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, and continue logical ammonia, temperature drops to less than 100 DEG C, takes out sample In 2si 6n 10: 0.03Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 8: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, passes into organic source (DPM) 3the mol ratio of In, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium is 2:6:0.06, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into ammonia, ammonia airshed is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, and continue logical ammonia, temperature drops to less than 100 DEG C, takes out sample In 2si 6n 10: 0.06Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 9: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, passes into organic source (DPM) 3the mol ratio of In, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium is 2:6:0.01, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into ammonia, ammonia airshed is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, and continue logical ammonia, temperature drops to less than 100 DEG C, takes out sample In 2si 6n 10: 0.01Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 10: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 4.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, passes into organic source (DPM) 3the mol ratio of Tl, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium is 2:6:0.03, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into ammonia, ammonia airshed is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, and continue logical ammonia, temperature drops to less than 100 DEG C, takes out sample Tl 2si 6n 10: 0.03Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 11: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, passes into organic source (DPM) 3the mol ratio of Tl, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium is 2:6:0.03, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into ammonia, ammonia airshed is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, and continue logical ammonia, temperature drops to less than 100 DEG C, takes out sample Tl 2si 6n 10: 0.06Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 12: substrate is the ito glass that Nan Bo company buys, and successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10 -2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, passes into organic source (DPM) 3the mol ratio of Tl, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium is 2:6:0.03, and gas of carrier gas is argon gas, and argon stream amount is 10sccm.Pass into ammonia, ammonia airshed is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, and continue logical ammonia, temperature drops to less than 100 DEG C, takes out sample Tl 2si 6n 10: 0.01Ce 3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.

Claims (10)

1. a cerium dopping Group III nitride silicon light-emitting film, is characterized in that, its chemical formula is Me 2si 6n 10: xCe 3+, wherein, 0.01≤x≤0.05, Me 2si 6n 10be matrix, Ce elements is active element, and Me is at least one in Al, Ga, In and Tl.
2. cerium dopping Group III nitride silicon light-emitting film according to claim 1, is characterized in that, the thickness of described cerium dopping Group III nitride silicon light-emitting film is 80nm ~ 300nm.
3. a preparation method for cerium dopping Group III nitride silicon light-emitting film, is characterized in that, comprise the following steps:
Substrate is loaded in the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10 -2pa ~ 1.0 × 10 -3pa;
Regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, adopts the carrier of argon stream, according to Me 2si 6n 10: xCe 3+the stoichiometric ratio of each element is by (DPM) 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium pass in reaction chamber; And
Pass into ammonia, carrying out chemical vapour deposition, to obtain chemical formula be Me 2si 6n 10: xCe 3+cerium dopping Group III nitride silicon light-emitting film, wherein, 0.01≤x≤0.05, Me 2si 6n 10be matrix, Ce elements is active element, and Me is at least one in Al, Ga, In and Tl.
4. the preparation method of cerium dopping Group III nitride silicon light-emitting film according to claim 3, is characterized in that, described (DPM) 3me, silane and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium mol ratio are 2:6:(0.01 ~ 0.05).
5. the preparation method of cerium dopping Group III nitride silicon light-emitting film according to claim 3, it is characterized in that, described argon stream amount is 5 ~ 15sccm.
6. the preparation method of cerium dopping Group III nitride silicon light-emitting film according to claim 3, is characterized in that, is loaded the thermal treatment 10 minutes ~ 30 minutes at 600 DEG C ~ 800 DEG C of described substrate by described substrate after described reaction chamber.
7. a membrane electro luminescent device, this membrane electro luminescent device comprises the substrate, anode layer, luminescent layer and the cathode layer that stack gradually, it is characterized in that, the material of described luminescent layer is cerium dopping Group III nitride silicon light-emitting film, and the chemical formula of this cerium dopping Group III nitride silicon light-emitting film is Me 2si 6n 10: xCe 3+, wherein, 0.01≤x≤0.05, Me 2si 6n 10be matrix, Ce elements is active element, and Me is at least one in Al, Ga, In and Tl.
8. membrane electro luminescent device according to claim 7, is characterized in that, the thickness of described luminescent layer is 80nm ~ 300nm.
9. a preparation method for membrane electro luminescent device, is characterized in that, comprises the following steps:
The substrate with anode is provided;
Described anode forms luminescent layer, and the film of described luminescent layer is cerium dopping Group III nitride silicon light-emitting film, and the chemical formula of this cerium dopping Group III nitride silicon light-emitting film is Me 2si 6n 10: xCe 3+, wherein, 0.01≤x≤0.05, Me 2si 6n 10be matrix, Ce elements is active element, and Me is at least one in Al, Ga, In and Tl;
Form negative electrode on the light-emitting layer.
10. the preparation method of membrane electro luminescent device according to claim 9, is characterized in that, the preparation of described luminescent layer comprises the following steps:
Described substrate is loaded the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10 -2pa ~ 1.0 × 10 -3pa;
Regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, adopts argon stream as carrier, according to Me 2si 6n 10: xCe 3+the stoichiometric ratio of each element is by (DPM) 3me, dipivaloylmethane yttrium, three molybdenum carbonyls, octafluoropentanol and four (acid of 2,2,6,6-tetramethyl--3,5-heptadione) cerium pass in reaction chamber, and wherein, argon stream amount is 5 ~ 15sccm,
Pass into ammonia, deposit film forms luminescent layer on described anode.
CN201310578442.XA 2013-11-18 2013-11-18 Cerium-doped three-family silicon nitride luminescence film, preparation method and application thereof Pending CN104650860A (en)

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Application publication date: 20150527