CN103805193A - Cerium-doped rare earth borate light-emitting film and preparation method and application thereof - Google Patents
Cerium-doped rare earth borate light-emitting film and preparation method and application thereof Download PDFInfo
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- CN103805193A CN103805193A CN201210459916.4A CN201210459916A CN103805193A CN 103805193 A CN103805193 A CN 103805193A CN 201210459916 A CN201210459916 A CN 201210459916A CN 103805193 A CN103805193 A CN 103805193A
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Abstract
The invention relates to a cerium-doped rare earth borate light-emitting film. The chemical formula of the cerium-doped rare earth borate light-emitting film is MeBO3:xCe<3+>, wherein x is more than or equal to 0.01 and less than or equal to 0.05, the MeBO3 is a matrix, a cerium element is an activated element, and Me is Y, La, Gd or Lu. The cerium-doped rare earth borate light-emitting film disclosed by the invention has very high light-emitting peaks in the 535 nanometer wavelength area of an EL (Electroluminescent Spectrum), thereby being applied to a film electroluminescent display. The invention also provides a preparation method and application of the cerium-doped rare earth borate light-emitting film.
Description
[technical field]
The present invention relates to rare earth doped borate light-emitting film of a kind of cerium and preparation method thereof and 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 luminous film of exploitation multiband, is the developing direction of this problem.But, can be applicable to the rare earth doped borate light-emitting film of cerium 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 rare earth doped borate light-emitting film of cerium that can be applicable to membrane electro luminescent device and preparation method thereof and membrane electro luminescent device and preparation method thereof.
The rare earth doped borate light-emitting film of a kind of cerium, its chemical formula is MeBO
3: xCe
3+, wherein MeBO
3be matrix, Ce elements is active element, 0.01≤x≤0.05, and Me is Y, La, Gd or Lu.
In a preferred embodiment, the thickness of the rare earth doped borate light-emitting film of cerium is 80nm～300nm.
A preparation method for the rare earth doped borate light-emitting film of cerium, comprises the following steps:
Substrate is packed 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;
Regulating substrate temperature is 250 ℃～650 ℃, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to MeBO
3: xCe
3+the stoichiometric ratio of each element is by Me (DPM)
3, BH
3pass in reaction chamber with dipivaloylmethane cerium, and
Then pass into oxygen, carrying out chemical vapour deposition, to obtain rare earth doped its chemical formula of borate light-emitting film of cerium be MeBO
3: xCe
3+, wherein MeBO
3be matrix, Ce elements is active element, 0.01≤x≤0.05, and Me is Y, La, Gd or Lu.
In a preferred embodiment, Me (DPM)
3, BH
3with dipivaloylmethane cerium mol ratio be 1: 1: (0.01～0.05).
In preferred embodiment, Me (DPM)
3, BH
3with dipivaloylmethane cerium mol ratio be 1: 1: 0.02.
In a preferred embodiment, argon stream amount is 5～15sccm, and oxygen flow amount 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 the rare earth doped borate light-emitting film of cerium, and the chemical formula of the rare earth doped borate light-emitting film of this cerium is MeBO
3: xCe
3+, wherein MeBO
3be matrix, Ce elements is active element, 0.01≤x≤0.05, and Me is Y, La, Gd or Lu.
In a preferred embodiment, the thickness of luminescent layer is 80nm～300nm.
A preparation method for membrane electro luminescent device, comprises the following steps:
The substrate with anode is provided;
On described anode, form luminescent layer, the material of described luminescent layer is the rare earth doped borate light-emitting film of cerium, and the chemical formula of the rare earth doped borate light-emitting film of this cerium is MeBO
3: xCe
3+, wherein MeBO
3be matrix, Ce elements is active element, 0.01≤x≤0.05, and Me is Y, La, Gd or Lu;
On described luminescent layer, form negative electrode.
In a preferred embodiment, the preparation of described luminescent layer comprises the following steps:
Substrate is packed 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;
Regulating substrate temperature is 250 ℃～650 ℃, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to MeBO
3: xCe
3+the stoichiometric ratio of each element is by Me (DPM)
3, BH
3pass in reaction chamber with dipivaloylmethane cerium, wherein, argon stream amount is 5～15sccm, and
Then pass into oxygen, flow is 10～200sccm; Carrying out chemical vapour deposition, to obtain luminescent layer chemical formula be MeBO
3: xCe
3+, wherein MeBO
3be matrix, Ce elements is active element, 0.01≤x≤0.05, and Me is Y, La, Gd or Lu.
The rare earth doped borate light-emitting film of above-mentioned cerium (MeBO
3: xCe
3+) electroluminescent spectrum (EL) in, have very strong glow peak in 535nm 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 the rare earth doped borate light-emitting film of cerium prepared of embodiment 1;
Fig. 3 is the XRD figure of the rare earth doped borate light-emitting film of cerium prepared of embodiment 1;
Fig. 4 is voltage and electric current and the brightness relationship figure of the membrane electro luminescent device prepared of embodiment 1.
[embodiment]
Below in conjunction with the drawings and specific embodiments, the rare earth doped borate light-emitting film of cerium, its preparation method and membrane electro luminescent device and preparation method thereof are further illustrated.
The rare earth doped borate light-emitting film of cerium of one embodiment, its chemical formula is MeBO
3: xCe
3+, wherein MeBO
3be matrix, Ce elements is active element, 0.01≤x≤0.05, and Me is Y, La, Gd or Lu.
Preferably, the thickness of the rare earth doped borate light-emitting film of cerium is 80nm～300nm, and x is 0.02.
MeBO in the rare earth doped borate light-emitting film of this cerium
3be matrix, Ce elements is active element.In the electroluminescent spectrum (EL) of the rare earth doped borate light-emitting film of this cerium, there is very strong glow peak in 535nm wavelength zone, can be applied in thin-film electroluminescent displays.
The preparation method of the rare earth doped borate light-emitting film of above-mentioned cerium, comprises the following steps:
Step S11, substrate is packed 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.
In the present embodiment, substrate is indium tin oxide glass (ITO), be appreciated that in other embodiments, also can be for fluorine doped tin oxide glass (FTO), mix the zinc oxide (AZO) of aluminium or mix the zinc oxide (IZO) of indium; Substrate is successively with toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into reaction chamber.
Preferably, the vacuum tightness of reaction chamber is 4.0 × 10
-3pa.
Step S12, by substrate thermal treatment 10 minutes～30 minutes at 600 ℃～800 ℃.
Step S13, adjusting substrate temperature are 250 ℃～650 ℃, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to MeBO
3: xCe
3+the stoichiometric ratio of each element is by Me (DPM)
3, BH
3pass in reaction chamber with dipivaloylmethane cerium.
In a preferred embodiment, Me (DPM)
3, BH
3with dipivaloylmethane cerium mol ratio be 1: 1: (0.01～0.05).
In preferred embodiment, Me (DPM)
3, BH
3with dipivaloylmethane cerium mol ratio be 1: 1: 0.02.
In a preferred embodiment, substrate temperature is preferably 500 ℃, 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 oxygen, carrying out chemical vapour deposition, to obtain rare earth doped its chemical formula of borate light-emitting film of cerium be MeBO
3: xCe
3+, wherein MeBO
3be matrix, Ce elements is active element, 0.01≤x≤0.05, and Me is Y, La, Gd or Lu.
In a preferred embodiment, oxygen flow amount is 10～200sccm, and x is 0.02.
In more preferred embodiment, oxygen flow amount is 120sccm.
After step S15, deposition, stop passing into Me (DPM)
3, BH
3with dipivaloylmethane cerium and argon gas, continue to pass into the temperature that oxygen makes the rare earth doped borate light-emitting film of cerium and be down to 80 ℃～150 ℃.
In present embodiment, preferred, make the temperature of the rare earth doped borate light-emitting film of cerium be down to 100 ℃.
Be appreciated that step S12 and step S15 can omit.
Refer to Fig. 1, the membrane electro luminescent device 100 of an embodiment, this membrane electro luminescent device 100 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 the rare earth doped borate light-emitting film of cerium, and the chemical formula of the rare earth doped borate light-emitting film of this cerium is MeBO
3: xCe
3+, wherein MeBO
3be matrix, Ce elements is active element, 0.01≤x≤0.05, and Me is Y, La, Gd or Lu.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, also can be for fluorine doped tin oxide glass (FTO), mix the zinc oxide (AZO) of aluminium or mix the zinc oxide (IZO) of indium; The substrate 1 with anode 2 is successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning and use it is carried out to oxygen plasma treatment.
Step S22, on anode 2, form luminescent layer 3, the material of luminescent layer 3 is the rare earth doped borate light-emitting film of cerium, and the chemical formula of the rare earth doped borate light-emitting film of this cerium is MeBO
3: xCe
3+, wherein MeBO
3be matrix, Ce elements is active element, 0.01≤x≤0.05, and Me is Y, La, Gd or Lu.
In present embodiment, luminescent layer 3 is made by following steps:
First, substrate is packed 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 ℃～800 ℃.Also can be without this step.
Secondly, regulating substrate temperature is 250 ℃～650 ℃, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to MeBO
3: xCe
3+the stoichiometric ratio of each element is by Me (DPM)
3, BH
3pass in reaction chamber with dipivaloylmethane cerium.
In a preferred embodiment, Me (DPM)
3, BH
3with dipivaloylmethane cerium mol ratio be 1: 1: (0.01～0.05).
In preferred embodiment, Me (DPM)
3, BH
3with dipivaloylmethane cerium mol ratio be 1: 1: 0.02.
In a preferred embodiment, substrate temperature is preferably 500 ℃, 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 oxygen, carry out chemical vapour deposition film and form luminescent layer on described anode.
In preferred embodiment, the flow of oxygen is preferably 10～200sccm.
In more preferred embodiment, oxygen flow amount is 120sccm.
Finally, after deposition, stop passing into Me (DPM)
3, BH
3with dipivaloylmethane cerium and argon gas, continue to pass into the temperature that oxygen makes the rare earth doped borate light-emitting film of cerium and be down to 80 ℃～150 ℃.
In present embodiment, preferred, make the temperature of the rare earth doped borate light-emitting film of cerium be down to 100 ℃.Can be without 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 uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 4.0 × 10 with mechanical pump and molecular pump
-3pa; Then substrate is carried out to 700 ℃ of thermal treatments 20 minutes, then temperature is reduced to 500 ℃.Open rotating machine, regulating the rotating speed of substrate bracket is 300 revs/min, passes into organic source dipivaloylmethane yttrium (Y (DPM)
3), borine (BH
3) and dipivaloylmethane cerium Ce (DPM)
4mol ratio be 1: 1: 0.02, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 ℃, takes out sample YBO
3: 0.02Ce
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula of the rare earth doped borate light-emitting film of cerium obtaining in the present embodiment is YBO
3: 0.02Ce
3+, wherein YBO
3be matrix, Ce elements is active element.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the rare earth doped borate light-emitting film of the cerium obtaining.As seen from Figure 2, in electroluminescence spectrum, there is very strong glow peak can be applied in thin-film electroluminescent displays in 535nm wavelength zone.
Refer to Fig. 3, Fig. 3 is the XRD curve of the rare earth doped borate light-emitting film of cerium prepared of embodiment 1, test comparison standard P DF card.From Fig. 3, reference standard PDF card, the diffraction peak in figure is the peak crystallization of RE(rare earth) borate, does not occur the diffraction peak of doped element and other impurity, illustrates that the product that this preparation method obtains has good crystalline quality.
Refer to Fig. 4, Fig. 4 is voltage and electric current and the brightness relationship figure of the membrane electro luminescent device prepared of embodiment 1, and in accompanying drawing 4, curve 1 is voltage and current density relation curve, can find out that device starts from 5.5V luminous, curve 2 is voltage and brightness relationship curve, and high-high brightness is 77cd/m
2, show that device has the good characteristics of luminescence.
Embodiment 2
Substrate is ito glass, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump
-3pa; Then substrate is carried out to 700 ℃ of thermal treatments 10 minutes, then temperature is reduced to 250 ℃.Open rotating machine, regulating the rotating speed of substrate bracket is 50 revs/min, passes into organic source dipivaloylmethane yttrium (Y (DPM)
3), borine (BH
3) and dipivaloylmethane cerium Ce (DPM)
4mol ratio be 1: 1: 0.05, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 ℃, takes out sample YBO
3: 0.05Ce
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 3
Substrate is ito glass, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump
-2pa; Then substrate is carried out to 700 ℃ of thermal treatments 30 minutes, then temperature is reduced to 650 ℃.Open rotating machine, regulating the rotating speed of substrate bracket is 1000 revs/min, passes into organic source dipivaloylmethane yttrium (Y (DPM)
3), borine (BH
3) and dipivaloylmethane cerium Ce (DPM)
4mol ratio be 1: 1: 0.01, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 ℃, takes out sample YBO
3: 0.01Ce
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 4: substrate is ito glass, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 4.0 × 10 with mechanical pump and molecular pump
-3pa; Then substrate is carried out to 700 ℃ of thermal treatments 20 minutes, then temperature is reduced to 500 ℃.Open rotating machine, regulating the rotating speed of substrate bracket is 300 revs/min, passes into organic source dipivaloylmethane lanthanum (La (DPM)
3), borine (BH
3) and dipivaloylmethane cerium Ce (DPM)
4mol ratio be 1: 1: 0.02, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 ℃, takes out sample LaBO
3: 0.02Ce
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, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump
-3pa; Then substrate is carried out to 700 ℃ of thermal treatments 10 minutes, then temperature is reduced to 250 ℃.Open rotating machine, regulating the rotating speed of substrate bracket is 50 revs/min, passes into organic source dipivaloylmethane lanthanum (La (DPM)
3), borine (BH
3) and dipivaloylmethane cerium Ce (DPM)
4mol ratio be 1: 1: 0.05, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 ℃, takes out sample LaBO
3: 0.05Ce
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, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump
-2pa; Then substrate is carried out to 700 ℃ of thermal treatments 30 minutes, then temperature is reduced to 650 ℃.Open rotating machine, regulating the rotating speed of substrate bracket is 1000 revs/min, passes into organic source dipivaloylmethane lanthanum (La (DPM)
3), borine (BH
3) and dipivaloylmethane cerium Ce (DPM)
4mol ratio be 1: 1: 0.01, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 ℃, takes out sample LaBO
3: 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, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 4.0 × 10 with mechanical pump and molecular pump
-3pa; Then substrate is carried out to 700 ℃ of thermal treatments 20 minutes, then temperature is reduced to 500 ℃.Open rotating machine, regulating the rotating speed of substrate bracket is 300 revs/min, passes into organic source dipivaloylmethane gadolinium (Gd (DPM)
3), borine (BH
3) and dipivaloylmethane cerium Ce (DPM)
4mol ratio be 1: 1: 0.02, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 ℃, takes out sample GdBO
3: 0.02Ce
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, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump
-3pa; Then substrate is carried out to 700 ℃ of thermal treatments 10 minutes, then temperature is reduced to 250 ℃.Open rotating machine, regulating the rotating speed of substrate bracket is 50 revs/min, passes into organic source dipivaloylmethane gadolinium (Gd (DPM)
3), borine (BH
3) and dipivaloylmethane cerium Ce (DPM)
4mol ratio be 1: 1: 0.05, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 ℃, takes out sample GdBO
3: 0.05Ce
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, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump
-2pa; Then substrate is carried out to 700 ℃ of thermal treatments 30 minutes, then temperature is reduced to 650 ℃.Open rotating machine, regulating the rotating speed of substrate bracket is 1000 revs/min, passes into organic source dipivaloylmethane gadolinium (Gd (DPM)
3), borine (BH
3) and dipivaloylmethane cerium Ce (DPM)
4mol ratio be 1: 1: 0.01, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 ℃, takes out sample GdBO
3: 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, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 4.0 × 10 with mechanical pump and molecular pump
-3pa; Then substrate is carried out to 700 ℃ of thermal treatments 20 minutes, then temperature is reduced to 500 ℃.Open rotating machine, regulating the rotating speed of substrate bracket is 300 revs/min, passes into organic source dipivaloylmethane lutetium (Lu (DPM)
3), borine (BH
3) and dipivaloylmethane cerium Ce (DPM)
4mol ratio be 1: 1: 0.02, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 120sccm, starts the deposition of film.The thickness of film is deposited into 150nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 ℃, takes out sample LuBO
3: 0.02Ce
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, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump
-3pa; Then substrate is carried out to 700 ℃ of thermal treatments 10 minutes, then temperature is reduced to 250 ℃.Open rotating machine, regulating the rotating speed of substrate bracket is 50 revs/min, passes into organic source dipivaloylmethane lutetium (Lu (DPM)
3), borine (BH
3) and dipivaloylmethane cerium Ce (DPM)
4mol ratio be 1: 1: 0.05, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 10sccm, starts the deposition of film.The thickness of film is deposited into 80nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 ℃, takes out sample LuBO
3: 0.05Ce
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, successively uses toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, after nitrogen is air-dry, sends into equipment reaction chamber.The vacuum tightness of cavity is evacuated to 1.0 × 10 with mechanical pump and molecular pump
-2pa; Then substrate is carried out to 700 ℃ of thermal treatments 30 minutes, then temperature is reduced to 650 ℃.Open rotating machine, regulating the rotating speed of substrate bracket is 1000 revs/min, passes into organic source dipivaloylmethane lutetium (Lu (DPM)
3), borine (BH
3) and dipivaloylmethane cerium Ce (DPM)
4mol ratio be 1: 1: 0.01, gas of carrier gas is argon gas, argon stream amount is 10sccm.Pass into oxygen, oxygen flow amount is 200sccm, starts the deposition of film.The thickness of film is deposited into 300nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to below 100 ℃, takes out sample LuBO
3: 0.01Ce
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore 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. the rare earth doped borate light-emitting film of cerium, is characterized in that, its chemical formula is MeBO
3: xCe
3+, wherein MeBO
3be matrix, Ce elements is active element, 0.01≤x≤0.05, and Me is Y, La, Gd or Lu.
2. the rare earth doped borate light-emitting film of cerium according to claim 1, is characterized in that, the thickness of the rare earth doped borate light-emitting film of described cerium is 80nm～300nm.
3. a preparation method for the rare earth doped borate light-emitting film of cerium, is characterized in that, comprises the following steps:
Substrate is packed 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;
Regulating substrate temperature is 250 ℃～650 ℃, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to MeBO
3: xCe
3+the stoichiometric ratio of each element is by Me (DPM)
3, BH
3pass in reaction chamber with dipivaloylmethane cerium; And
Pass into oxygen, carrying out chemical vapour deposition, to obtain chemical formula be MeBO
3: xCe
3+the rare earth doped borate light-emitting film of cerium, wherein MeBO
3be matrix, Ce elements is active element, 0.01≤x≤0.05, and Me is Y, La, Gd or Lu.
4. the preparation method of the rare earth doped borate light-emitting film of cerium according to claim 3, is characterized in that, described Me (DPM)
3, BH
3with dipivaloylmethane cerium mol ratio be 1: 1: (0.01～0.05).
5. the preparation method of the rare earth doped borate light-emitting film of cerium according to claim 3, is characterized in that, described argon stream amount is 5sccm～15sccm, and described oxygen flow amount is 10sccm～200sccm.
6. the preparation method of the rare earth doped borate light-emitting film of cerium according to claim 3, is characterized in that, described substrate is packed into after described reaction chamber the thermal treatment 10 minutes～30 minutes at 600 ℃～800 ℃ of described substrate.
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 the rare earth doped borate light-emitting film of cerium, and the chemical formula of the rare earth doped borate light-emitting film of this cerium is MeBO
3: xCe
3+, wherein MeBO
3be matrix, Ce elements is active element, 0.01≤x≤0.05, and Me is Y, La, Gd or Lu.
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;
On described anode, form luminescent layer, the film of described luminescent layer is the rare earth doped borate light-emitting film of cerium, and the chemical formula of the rare earth doped borate light-emitting film of this cerium is MeBO
3: xCe
3+, wherein MeBO
3be matrix, Ce elements is active element, 0.01≤x≤0.05, and Me is Y, La, Gd or Lu;
On described luminescent layer, form negative electrode.
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 packed into 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;
Regulating substrate temperature is 250 ℃～650 ℃, and rotating speed is 50 revs/min～1000 revs/min, adopts argon stream as carrier, according to MeBO
3: xCe
3+the stoichiometric ratio of each element is by Me (DPM)
3, BH
3pass in reaction chamber with dipivaloylmethane cerium, wherein, argon stream amount is 5sccm～15sccm,
Then pass into oxygen, oxygen flow amount is 10sccm～200sccm; Deposit film forms luminescent layer on described anode.
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