CN103421494B - Titanium magnesium codoped alumina luminescent thin film, preparation method and applications - Google Patents
Titanium magnesium codoped alumina luminescent thin film, preparation method and applications Download PDFInfo
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Abstract
A kind of titanium magnesium codoped alumina luminescent thin film, its chemical formula is Al2O3:xTi4+, yMg2+, wherein aluminium oxide is substrate, and titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06.In the electroluminescent spectrum (EL) of this titanium magnesium codoped alumina luminescent thin film, there is the strongest glow peak in 410nm wavelength zone, it is possible to be applied in thin-film electroluminescent displays.The present invention also provides for the preparation method and applications of this titanium magnesium codoped alumina luminescent thin film.
Description
[technical field]
The present invention relates to a kind of titanium magnesium codoped alumina luminescent thin film, its preparation method, TFEL
Device and preparation method thereof.
[background technology]
Thin-film electroluminescent displays (TFELD) owing to its active illuminating, total solids, impact resistance, reaction are fast,
The advantages such as visual angle is big, Applicable temperature width, operation are simple, have caused and have paid close attention to widely, and quickly grown.
At present, studying colored and extremely panchromatic TFELD, the thin film that exploitation multiband is luminous, is the development side of this problem
To.But, can be applicable to the titanium magnesium codoped alumina luminescent thin film of thin-film electroluminescent displays, not yet
Appear in the newspapers.
[summary of the invention]
Based on this, it is necessary to provide a kind of titanium magnesium codope aluminium oxide that can be applicable to membrane electro luminescent device
Light-emitting film, its preparation method this titanium magnesium codoped alumina luminescent thin film electroluminescent device and preparation side thereof
Method.
A kind of titanium magnesium codoped alumina luminescent thin film, its chemical formula is Al2O3:xTi4+, yMg2+, wherein,
Aluminium oxide is substrate, and titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06.
In a preferred embodiment, the thickness of titanium magnesium codoped alumina luminescent thin film is 80nm～300nm.
The preparation method of a kind of titanium magnesium codoped alumina luminescent thin film, comprises the following steps:
Substrate is loaded in the reative cell of chemical vapor depsotition equipment, and the vacuum of reative cell is set to
1.0×10-2Pa～1.0 × 10-3Pa；
Regulation substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, uses argon
The carrier of entraining air stream, according to Al2O3:xTi4+, yMg2+The stoichiometric proportion of each element by triethyl aluminum, four
Isopropyl titanate and two cyclopentadienyl magnesium are passed through in reative cell, and
Then pass to oxygen, carry out chemical gaseous phase deposition and obtain its chemistry of titanium magnesium codoped alumina luminescent thin film
Formula is Al2O3:xTi4+, yMg2+, wherein, aluminium oxide is substrate, and titanium elements and magnesium elements are active elements,
0.01≤x≤0.08,0≤y≤0.06.
In a preferred embodiment, triethyl aluminum, titanium tetraisopropylate and two cyclopentadienyl magnesium mol ratios are 1:
(0.01～0.08): (0～0.06)；
In a more preferred embodiment, triethyl aluminum, titanium tetraisopropylate and two cyclopentadienyl magnesium mol ratios are 1: 0.05:
0.03,
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 includes substrate, the anode stacked gradually
Layer, luminescent layer and cathode layer, the material of described luminescent layer is titanium magnesium codoped alumina luminescent thin film, should
The chemical formula of titanium magnesium codoped alumina luminescent thin film is Al2O3:xTi4+, yMg2+, wherein, aluminium oxide is
Substrate, titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06.
The preparation method of a kind of membrane electro luminescent device, comprises the following steps:
The substrate with anode is provided；
Forming luminescent layer on described anode, the material of described luminescent layer is that titanium magnesium codope aluminium oxide luminescence is thin
Film, the chemical formula of this titanium magnesium codoped alumina luminescent thin film is Al2O3:xTi4+, yMg2+, wherein, oxygen
Changing aluminum is substrate, and titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06；
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 reative cell of chemical vapor depsotition equipment, and the vacuum of reative cell is set to
1.0×10-2Pa～1.0 × 10-3Pa；
Regulation substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, uses argon
The carrier of entraining air stream, according to Al2O3:xTi4+, yMg2+The stoichiometric proportion of each element by triethyl aluminum, four
Isopropyl titanate and two cyclopentadienyl magnesium are passed through in reative cell, and wherein, argon stream amount is 5～15sccm, and
Then passing to oxygen, flow is 10～200sccm；Carry out chemical gaseous phase deposition and obtain luminescent layer chemical formula
For Al2O3:xTi4+, yMg2+, wherein, aluminium oxide is substrate, and titanium elements and magnesium elements are active elements,
0.01≤x≤0.08,0≤y≤0.06.
Above-mentioned titanium magnesium codoped alumina luminescent thin film (Al2O3:xTi4+, yMg2+) electroluminescent spectrum
(EL) in, there is the strongest glow peak in 410nm wavelength zone, it is possible to be applied to TFEL and show
In device.
[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 titanium magnesium codoped alumina luminescent thin film of embodiment 1 preparation；
Fig. 3 is the XRD figure of the titanium magnesium codoped alumina luminescent thin film of embodiment 1 preparation；
Fig. 4 is voltage and electric current and the brightness relationship figure of the membrane electro luminescent device of embodiment 1 preparation.
[detailed description of the invention]
Below in conjunction with the accompanying drawings with specific embodiment to titanium magnesium codoped alumina luminescent thin film, its preparation method and
Membrane electro luminescent device and preparation method thereof is further elucidated with.
The titanium magnesium codoped alumina luminescent thin film of one embodiment, its chemical formula is Al2O3:xTi4+, yMg2+,
Wherein, aluminium oxide is substrate, and titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06.
Preferably, the thickness of titanium magnesium codoped alumina luminescent thin film is 80nm～300nm, and x is 0.05, y
It is 0.03.
In this titanium magnesium codoped alumina luminescent thin film, aluminium oxide is substrate, and titanium elements and magnesium elements are to activate unit
Element.In the electroluminescent spectrum (EL) of this titanium magnesium codoped alumina luminescent thin film, in 410nm wavelength zone
There is the strongest glow peak, it is possible to be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned titanium magnesium codoped alumina luminescent thin film, comprises the following steps:
Step S11, substrate is loaded in the reative cell of chemical vapor depsotition equipment, and by the vacuum of reative cell
It is set to 1.0 × 10-2Pa～1.0 × 10-3Pa。
In the present embodiment, substrate is indium tin oxide glass (ITO), it will be understood that implement at other
In example, it is also possible to the zinc oxide (AZO) for fluorine doped tin oxide glass (FTO), mixing aluminum or indium-doped oxidation
Zinc (IZO)；Substrate successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then uses distilled water flushing
Totally, reative cell is sent into after nitrogen air-dries；
Preferably, the vacuum of reative cell is 4.0 × 10-3Pa。
Step S12, by substrate heat treatment 10 minutes～30 minutes at 600 DEG C～800 DEG C.
Step S13, regulation substrate temperature are 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min
Clock, uses the carrier of argon stream, according to Al2O3:xTi4+, yMg2+The stoichiometric proportion of each element is by three
Aluminium ethide, titanium tetraisopropylate and two cyclopentadienyl magnesium are passed through in reative cell；
In a preferred embodiment, triethyl aluminum, titanium tetraisopropylate and two cyclopentadienyl magnesium mol ratios are 1:
(0.01～0.08): (0～0.06)；
In a more preferred embodiment, triethyl aluminum, titanium tetraisopropylate and two cyclopentadienyl magnesium mol ratios are 1: 0.05:
0.03,
In a preferred embodiment, substrate temperature is preferably 500 DEG C, and the rotating speed of substrate is preferably 300 revs/min
Clock, argon stream amount is 5～15sccm；
In more preferred embodiment, argon stream amount is 10sccm；
Step S14, then passing to oxygen, carrying out chemical gaseous phase deposition, to obtain titanium magnesium codope aluminium oxide luminescence thin
Its chemical formula of film is Al2O3:xTi4+, yMg2+, wherein, aluminium oxide is substrate, and titanium elements and magnesium elements are
Active element, 0.01≤x≤0.08,0≤y≤0.06.
In a preferred embodiment, oxygen flow amount is 10～200sccm, and x is 0.05, and y is 0.03.
In more preferred embodiment, oxygen flow amount is 120sccm.
Stop after step S15, deposition being passed through triethyl aluminum, titanium tetraisopropylate and two cyclopentadienyl magnesium and argon, continue
Continuous it be passed through oxygen and make the temperature of titanium magnesium codoped alumina luminescent thin film be down to 80 DEG C～150 DEG C.
In present embodiment, it is preferred that make the temperature of titanium magnesium codoped alumina luminescent thin film be down to 100 DEG C.
It is appreciated that step S12 and step S15 can be omitted.
Refer to Fig. 1, the membrane electro luminescent device 100 of an embodiment, this membrane electro luminescent device 100
Including the substrate 1 stacked gradually, anode 2, luminescent layer 3 and negative electrode 4.
Substrate 1 is glass substrate.Anode 2 is the tin indium oxide (ITO) being formed in glass substrate.Luminous
The material of layer 3 is titanium magnesium codoped alumina luminescent thin film, the change of this titanium magnesium codoped alumina luminescent thin film
Formula is Al2O3:xTi4+, yMg2+, wherein, aluminium oxide is substrate, and titanium elements and magnesium elements are to activate unit
Element, 0.01≤x≤0.08,0≤y≤0.06.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, offer have the substrate 1 of anode 2.
In present embodiment, substrate 1 is glass substrate, and anode 2 is the Indium sesquioxide. being formed in glass substrate
Stannum (ITO).It is appreciated that in other embodiments, it is also possible to for fluorine doped tin oxide glass (FTO), mix
The zinc oxide (AZO) of aluminum or indium-doped zinc oxide (IZO)；Have anode 2 substrate 1 priority acetone,
Dehydrated alcohol and deionized water ultrasonic cleaning also carry out oxygen plasma treatment with to it.
Step S22, on anode 2 formed luminescent layer 3, the material of luminescent layer 3 is titanium magnesium codope aluminium oxide
Light-emitting film, the chemical formula of this titanium magnesium codoped alumina luminescent thin film is Al2O3:xTi4+, yMg2+, its
Middle aluminium oxide is substrate, and titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06.
In present embodiment, luminescent layer 3 is prepared by following steps:
First, substrate is loaded in the reative cell of chemical vapor depsotition equipment, and the vacuum of reative cell is set
It is set to 1.0 × 10-2Pa～1.0 × 10-3Pa,
Moreover, by substrate heat treatment 10 minutes～30 minutes at 600 DEG C～800 DEG C.Can also walk without this
Suddenly.
Secondly, regulation substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min,
Use the carrier of argon stream, according to Al2O3:xTi4+, yMg2+The stoichiometric proportion of each element is by triethyl group
Aluminum, titanium tetraisopropylate and two cyclopentadienyl magnesium are passed through in reative cell；
In a preferred embodiment, triethyl aluminum, titanium tetraisopropylate and two cyclopentadienyl magnesium mol ratios are 1:
(0.01～0.08): (0～0.06)；
In a more preferred embodiment, triethyl aluminum, titanium tetraisopropylate and two cyclopentadienyl magnesium mol ratios are 1: 0.05:
0.03,
In a preferred embodiment, substrate temperature is preferably 500 DEG C, and the rotating speed of substrate is preferably 300 revs/min
Clock, argon stream amount is 5～15sccm；
In more preferred embodiment, argon stream amount is 10sccm；
Then pass to oxygen, carry out chemical vapour deposition film on described anode, form luminescent layer.
In preferred embodiment, the flow of oxygen is preferably 10～200sccm；
In more preferred embodiment, oxygen flow amount is 120sccm.
Finally, stop after deposition being passed through triethyl aluminum, titanium tetraisopropylate and two cyclopentadienyl magnesium and argon, continuation
Being passed through oxygen makes the temperature of titanium magnesium codoped alumina luminescent thin film be down to 80 DEG C～150 DEG C.
In present embodiment, it is preferred that make the temperature of titanium magnesium codoped alumina luminescent thin film be down to 100 DEG C.
Can be without this step.
Step S23, on luminescent layer 3 formed negative electrode 4.
In present embodiment, the material of negative electrode 4 is silver (Ag), evaporation formed.
It is specific embodiment below.
Embodiment 1
Substrate is ito glass, successively cleans 5 minutes, then with distillation with toluene, acetone and EtOH Sonicate
Water is rinsed well, and nitrogen sends into equipment reaction chamber after air-drying.With mechanical pump and molecular pump the vacuum of cavity
It is evacuated to 4.0 × 10-3Pa；Then substrate being carried out 700 DEG C of heat treatments 20 minutes, then temperature reduces to 500 DEG C.
Opening electric rotating machine, the rotating speed of regulation substrate bracket is 300 revs/min, is passed through organic source triethyl aluminum
(CH3CH2)3Al, titanium tetraisopropylate TTIP and two cyclopentadienyl magnesium (C5H5)2The mol ratio of Mg is 1: 0.05: 0.03,
Gas of carrier gas is argon, and argon stream amount is 10sccm.Being passed through oxygen, oxygen flow amount is 120sccm,
Start the deposition of thin film.The thickness of thin film deposits to 150nm, closes organic source and carrier gas, continues logical oxygen,
Temperature drops to less than 100 DEG C, takes out sample Al2O3:0.05Ti4+, 0.03Mg2+.Last on light-emitting film
Face one layer of Ag of evaporation, as negative electrode.
The chemical general formula of the titanium magnesium codoped alumina luminescent thin film obtained in the present embodiment is Al2O3:
0.05Ti4+, 0.03Mg2+, wherein aluminium oxide is substrate, and titanium elements and magnesium elements are active elements.
Refer to Fig. 2, Fig. 2 and show the electroluminescence spectrum of the titanium magnesium codoped alumina luminescent thin film obtained
(EL).As seen from Figure 2, in electroluminescence spectrum, there is the strongest glow peak in 410nm wavelength zone
Can be applied in thin-film electroluminescent displays.
The XRD referring to the titanium magnesium codoped alumina luminescent thin film that Fig. 3, Fig. 3 are embodiment 1 preparation is bent
Line, test comparison standard PDF card.The most all of diffraction maximum can be seen that all of spreading out
Penetrate the crystallization phase that peak is all corresponding aluminium oxide, and do not have doped chemical and other dephasign to occur, illustrate that this is prepared
The product that method obtains has good crystalline quality.
Refer to voltage and electric current and the brightness of the membrane electro luminescent device that Fig. 4, Fig. 4 are embodiment 1 preparation
Graph of a relation, curve 1 is voltage and electric current density relation curve in figure 4, it can be seen that device is opened from 5.5V
Originating light, curve 2 is voltage and brightness relationship curve, and high-high brightness is 79cd/m2, show that device has good
The good characteristics of luminescence.
Embodiment 2
Substrate is ito glass, successively cleans 5 minutes, then with distillation with toluene, acetone and EtOH Sonicate
Water is rinsed well, and nitrogen sends into equipment reaction chamber after air-drying.With mechanical pump and molecular pump the vacuum of cavity
It is evacuated to 1.0 × 10-3Pa；Then substrate being carried out 700 DEG C of heat treatments 10 minutes, then temperature reduces to 250 DEG C.
Opening electric rotating machine, the rotating speed of regulation substrate bracket is 50 revs/min, is passed through organic source triethyl aluminum
(CH3CH2)3Al, titanium tetraisopropylate TTIP and two cyclopentadienyl magnesium (C5H5)2The mol ratio of Mg is 1: 0.08: 0.06,
Gas of carrier gas is argon, and argon stream amount is 10sccm.Being passed through oxygen, oxygen flow amount is 10sccm, opens
The deposition of beginning thin film.The thickness of thin film deposits to 80nm, closes organic source and carrier gas, continues logical oxygen, temperature
Degree drops to less than 100 DEG C, takes out sample Al2O3:0.08Ti4+, 0.06Mg2+.Last on light-emitting film
It is deposited with one layer of Ag, as negative electrode.
Embodiment 3
Substrate is ito glass, successively cleans 5 minutes, then with distillation with toluene, acetone and EtOH Sonicate
Water is rinsed well, and nitrogen sends into equipment reaction chamber after air-drying.With mechanical pump and molecular pump the vacuum of cavity
It is evacuated to 1.0 × 10-2Pa；Then substrate being carried out 700 DEG C of heat treatments 30 minutes, then temperature reduces to 650 DEG C.
Opening electric rotating machine, the rotating speed of regulation substrate bracket is 1000 revs/min, is passed through organic source triethyl aluminum
(CH3CH2)3The mol ratio of Al and titanium tetraisopropylate TTIP is 1: 0.01, and gas of carrier gas is argon, argon gas
Flow is 10sccm.Being passed through oxygen, oxygen flow amount is 200sccm, starts the deposition of thin film.Thin film
Thickness deposits to 300nm, closes organic source and carrier gas, continues logical oxygen, and temperature drops to less than 100 DEG C, takes
Go out sample Al2O3:0.01Ti4+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment 4
Substrate is ito glass, successively cleans 5 minutes, then with distillation with toluene, acetone and EtOH Sonicate
Water is rinsed well, and nitrogen sends into equipment reaction chamber after air-drying.With mechanical pump and molecular pump the vacuum of cavity
It is evacuated to 1.0 × 10-3Pa；Then substrate being carried out 700 DEG C of heat treatments 10 minutes, then temperature reduces to 300 DEG C.
Opening electric rotating machine, the rotating speed of regulation substrate bracket is 200 revs/min, is passed through organic source triethyl aluminum
(CH3CH2)3Al, titanium tetraisopropylate TTIP and two cyclopentadienyl magnesium (C5H5)2The mol ratio of Mg is 1: 0.03: 0.02,
Gas of carrier gas is argon, and argon stream amount is 20sccm.Being passed through oxygen, oxygen flow amount is 100sccm,
Start the deposition of thin film.The thickness of thin film deposits to 150nm, closes organic source and carrier gas, continues logical oxygen,
Temperature drops to less than 100 DEG C, takes out sample Al2O3:0.03Ti4+, 0.02Mg2+.Last on light-emitting film
Face one layer of Ag of evaporation, as negative electrode.
Embodiment 5
Substrate is ito glass, successively cleans 5 minutes, then with distillation with toluene, acetone and EtOH Sonicate
Water is rinsed well, and nitrogen sends into equipment reaction chamber after air-drying.With mechanical pump and molecular pump the vacuum of cavity
It is evacuated to 1.0 × 10-3Pa；Then substrate being carried out 700 DEG C of heat treatments 10 minutes, then temperature reduces to 300 DEG C.
Opening electric rotating machine, the rotating speed of regulation substrate bracket is 200 revs/min, is passed through organic source triethyl aluminum
(CH3CH2)3Al, titanium tetraisopropylate TTIP and two cyclopentadienyl magnesium (C5H5)2The mol ratio of Mg is 1: 0.04: 0.04,
Gas of carrier gas is argon, and argon stream amount is 20sccm.Being passed through oxygen, oxygen flow amount is 100sccm,
Start the deposition of thin film.The thickness of thin film deposits to 150nm, closes organic source and carrier gas, continues logical oxygen,
Temperature drops to less than 100 DEG C, takes out sample Al2O3:0.04Ti4+, 0.04Mg2+.Last on light-emitting film
Face one layer of Ag of evaporation, as negative electrode.
Embodiment 6
Substrate is ito glass, successively cleans 5 minutes, then with distillation with toluene, acetone and EtOH Sonicate
Water is rinsed well, and nitrogen sends into equipment reaction chamber after air-drying.With mechanical pump and molecular pump the vacuum of cavity
It is evacuated to 1.0 × 10-3Pa；Then substrate being carried out 700 DEG C of heat treatments 10 minutes, then temperature reduces to 300 DEG C.
Opening electric rotating machine, the rotating speed of regulation substrate bracket is 200 revs/min, is passed through organic source triethyl aluminum
(CH3CH2)3Al, titanium tetraisopropylate TTIP and two cyclopentadienyl magnesium (C5H5)2The mol ratio of Mg is 1: 0.02: 0.01,
Gas of carrier gas is argon, and argon stream amount is 20sccm.Being passed through oxygen, oxygen flow amount is 100sccm,
Start the deposition of thin film.The thickness of thin film deposits to 150nm, closes organic source and carrier gas, continues logical oxygen,
Temperature drops to less than 100 DEG C, takes out sample Al2O3:0.02Ti4+, 0.01Mg2+.Last on light-emitting film
Face one layer of Ag of evaporation, as negative electrode.
Embodiment 7
Substrate is ito glass, successively cleans 5 minutes, then with distillation with toluene, acetone and EtOH Sonicate
Water is rinsed well, and nitrogen sends into equipment reaction chamber after air-drying.With mechanical pump and molecular pump the vacuum of cavity
It is evacuated to 1.0 × 10-3Pa；Then substrate being carried out 700 DEG C of heat treatments 10 minutes, then temperature reduces to 300 DEG C.
Opening electric rotating machine, the rotating speed of regulation substrate bracket is 200 revs/min, is passed through organic source triethyl aluminum
(CH3CH2)3Al, titanium tetraisopropylate TTIP and two cyclopentadienyl magnesium (C5H5)2The mol ratio of Mg is 1: 0.06: 0.04,
Gas of carrier gas is argon, and argon stream amount is 20sccm.Being passed through oxygen, oxygen flow amount is 100sccm,
Start the deposition of thin film.The thickness of thin film deposits to 150nm, closes organic source and carrier gas, continues logical oxygen,
Temperature drops to less than 100 DEG C, takes out sample Al2O3:0.06Ti4+, 0.04Mg2+.Last on light-emitting film
Face one layer of Ag of evaporation, as negative electrode.
Embodiment 8
Substrate is ito glass, successively cleans 5 minutes, then with distillation with toluene, acetone and EtOH Sonicate
Water is rinsed well, and nitrogen sends into equipment reaction chamber after air-drying.With mechanical pump and molecular pump the vacuum of cavity
It is evacuated to 1.0 × 10-3Pa；Then substrate being carried out 700 DEG C of heat treatments 10 minutes, then temperature reduces to 300 DEG C.
Opening electric rotating machine, the rotating speed of regulation substrate bracket is 200 revs/min, is passed through organic source triethyl aluminum
(CH3CH2)3Al, titanium tetraisopropylate TTIP and two cyclopentadienyl magnesium (C5H5)2The mol ratio of Mg is 1: 0.07: 0.05,
Gas of carrier gas is argon, and argon stream amount is 20sccm.Being passed through oxygen, oxygen flow amount is 100sccm,
Start the deposition of thin film.The thickness of thin film deposits to 150nm, closes organic source and carrier gas, continues logical oxygen,
Temperature drops to less than 100 DEG C, takes out sample Al2O3:0.07Ti4+, 0.05Mg2+.Last on light-emitting film
Face one layer of Ag of evaporation, as negative electrode.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more 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 this area
Those of ordinary skill for, without departing from the inventive concept of the premise, it is also possible to make some deformation and
Improving, these broadly fall into protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be with appended
Claim is as the criterion.
Claims (7)
1. the preparation method of a titanium magnesium codoped alumina luminescent thin film, it is characterised in that include following step
Rapid:
Substrate is loaded in the reative cell of chemical vapor depsotition equipment, and the vacuum of reative cell is set to
1.0×10-2Pa～1.0 × 10-3Pa；
Regulation substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, uses argon
The carrier of entraining air stream, according to Al2O3: xTi4+, yMg2+The stoichiometric proportion of each element by triethyl aluminum, four
Isopropyl titanate and two cyclopentadienyl magnesium are passed through in reative cell；And
Being passed through oxygen, carrying out chemical gaseous phase deposition and obtaining chemical formula is Al2O3: xTi4+, yMg2+Titanium magnesium altogether
Doped aluminium light-emitting film, wherein, aluminium oxide is substrate, and titanium elements and magnesium elements are active elements,
0.01≤x≤0.08,0 ＜ y≤0.06.
The preparation method of titanium magnesium codoped alumina luminescent thin film the most according to claim 1, its feature
Being, described triethyl aluminum, titanium tetraisopropylate and two cyclopentadienyl magnesium mol ratios are 1:x:y, 0.01≤x≤0.08,0 ＜
y≤0.06。
The preparation method of titanium magnesium codoped alumina luminescent thin film the most according to claim 1, its feature
Being, described argon stream amount is 5～15sccm, and described oxygen flow amount is 10～200sccm.
The preparation method of titanium magnesium codoped alumina luminescent thin film the most according to claim 1, its feature
It is, described substrate is loaded described substrate heat treatment 10 points at 600 DEG C～800 DEG C after described reative cell
Clock～30 minutes.
5. the preparation method of a titanium doped alumina luminescent thin film, it is characterised in that comprise the following steps:
Substrate is loaded in the reative cell of chemical vapor depsotition equipment, and the vacuum of reative cell is set to
1.0×10-2Pa～1.0 × 10-3Pa；
Regulation substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, uses argon
The carrier of entraining air stream, according to Al2O3: xTi4+The stoichiometric proportion of each element is by triethyl aluminum and titanium tetraisopropylate
It is passed through in reative cell；And
Being passed through oxygen, carrying out chemical gaseous phase deposition and obtaining chemical formula is Al2O3: xTi4+Titanium doped aluminium oxide send out
Optical thin film, wherein, aluminium oxide is substrate, and titanium elements is active element, 0.01≤x≤0.08.
6. the preparation method of a membrane electro luminescent device, it is characterised in that comprise the following steps:
The substrate with anode is provided；
Forming luminescent layer on described anode, the thin film of described luminescent layer is that titanium magnesium codope aluminium oxide luminescence is thin
Film, the chemical formula of this titanium magnesium codoped alumina luminescent thin film is Al2O3: xTi4+, yMg2+, wherein, oxygen
Changing aluminum is substrate, and titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0 ＜ y≤0.06；Described luminescence
The preparation of layer comprises the following steps:
Described substrate is loaded the reative cell of chemical vapor depsotition equipment, and the vacuum of reative cell is set to
1.0×10-2Pa～1.0 × 10-3Pa；
Regulation substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, uses argon
Entraining air stream is as carrier, according to Al2O3: xTi4+, yMg2+The stoichiometric proportion of each element by triethyl aluminum,
Titanium tetraisopropylate and two cyclopentadienyl magnesium are passed through in reative cell, and wherein, argon stream amount is 5～15sccm,
Then passing to oxygen, oxygen flow amount is 10～200sccm；Deposition thin film is formed on described anode to be sent out
Photosphere；
Form negative electrode on the light-emitting layer.
7. the preparation method of a membrane electro luminescent device, it is characterised in that comprise the following steps:
The substrate with anode is provided；
Forming luminescent layer on described anode, the thin film of described luminescent layer is titanium doped alumina luminescent thin film,
The chemical formula of this titanium doped alumina luminescent thin film is Al2O3: xTi4+, wherein, aluminium oxide is substrate, titanium unit
Element is active element, 0.01≤x≤0.08；The preparation of described luminescent layer comprises the following steps:
Described substrate is loaded the reative cell of chemical vapor depsotition equipment, and the vacuum of reative cell is set to
1.0×10-2Pa～1.0 × 10-3Pa；
Regulation substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, uses argon
Entraining air stream is as carrier, according to Al2O3: xTi4+The stoichiometric proportion of each element is by triethyl aluminum and four isopropanols
Titanium is passed through in reative cell, and wherein, argon stream amount is 5～15sccm,
Then passing to oxygen, oxygen flow amount is 10～200sccm；Deposition thin film is formed on described anode to be sent out
Photosphere；
Form negative electrode on the light-emitting layer.
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| US5064461A (en) * | 1990-10-29 | 1991-11-12 | Corning Incorporated | Blue/gray transparent glass-ceramic articles |
| CN1727303A (en) * | 2005-06-29 | 2006-02-01 | 上海大学 | Method for fabricating Mg, Ti adulterated Al2O3 crystalline material, and transparent laser ceramics |
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| Charge-exchange processes in titanium-doped sapphire crystals I. Charge-exchange energies and titanium-bound excitons;Wing C.Wong等;《PHYSICAL REVIEW B》;19950301;第51卷(第9期);第5682-5692 * |
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