CN103421494A - Titanium and magnesium codoped alumina luminescent thin film and preparation method and application thereof - Google Patents
Titanium and magnesium codoped alumina luminescent thin film and preparation method and application thereof Download PDFInfo
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- CN103421494A CN103421494A CN2012101512046A CN201210151204A CN103421494A CN 103421494 A CN103421494 A CN 103421494A CN 2012101512046 A CN2012101512046 A CN 2012101512046A CN 201210151204 A CN201210151204 A CN 201210151204A CN 103421494 A CN103421494 A CN 103421494A
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Abstract
A titanium and magnesium codoped alumina luminescent thin film has a chemical formula of Al2O3:xTi<4+>, yMg<2+>, wherein alumina is a matrix, titanium element and magnesium element are activation elements, x is greater than or equal to 0.01 and is less than or equal to 0.08, and y is greater than or equal to 0 and is less than or equal to 0.06. In an electroluminescence (EL) spectrum of the titanium and magnesium codoped alumina luminescent thin film, a wavelength region of 410 nm has very strong luminescence peaks, and the titanium and magnesium codoped alumina luminescent thin film can be used in a thin-film electroluminescent display. The invention also provides a preparation method and application of the titanium and magnesium codoped alumina luminescent thin film.
Description
[technical field]
The present invention relates to a kind of titanium magnesium codoped aluminum oxide 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 is colored to be reached to panchromatic TFELD, and the luminous film of exploitation multiband, be the developing direction of this problem.But, can be applicable to the titanium magnesium codoped aluminum oxide 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 titanium magnesium codoped aluminum oxide light-emitting film that can be applicable to membrane electro luminescent device, this titanium magnesium codoped aluminum oxide light-emitting film electroluminescent device of its preparation method and preparation method thereof.
A kind of titanium magnesium codoped aluminum oxide light-emitting film, its chemical formula is Al
2O
3: xTi
4+, yMg
2+, wherein, aluminum oxide is matrix, 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 aluminum oxide light-emitting film is 80nm～300nm.
A kind of preparation method of titanium magnesium codoped aluminum oxide light-emitting film 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 rev/mins～1000 rev/mins, adopts the carrier of argon stream, according to Al
2O
3: xTi
4+, yMg
2+The stoichiometric ratio of each element passes into triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium in reaction chamber, and
Then pass into oxygen, carrying out chemical vapour deposition, to obtain its chemical formula of titanium magnesium codoped aluminum oxide light-emitting film be Al
2O
3: xTi
4+, yMg
2+, wherein, aluminum oxide is matrix, 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 luxuriant magnesium mol ratios are 1: (0.01～0.08): (0～0.06);
In preferred embodiment, triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium mol ratios are 1: 0.05: 0.03,
In a preferred embodiment, the argon stream amount is 5～15sccm, and the oxygen flow amount is 10～200sccm.
A kind of membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer stacked gradually, the material of described luminescent layer is titanium magnesium codoped aluminum oxide light-emitting film, and the chemical formula of this titanium magnesium codoped aluminum oxide light-emitting film is Al
2O
3: xTi
4+, yMg
2+, wherein, aluminum oxide is matrix, titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06.
A kind of preparation method of membrane electro luminescent device comprises the following steps:
Substrate with anode is provided;
Form luminescent layer on described anode, the material of described luminescent layer is titanium magnesium codoped aluminum oxide light-emitting film, and the chemical formula of this titanium magnesium codoped aluminum oxide light-emitting film is Al
2O
3: xTi
4+, yMg
2+, wherein, aluminum oxide is matrix, titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06;
Form negative electrode on described luminescent layer.
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 rev/mins～1000 rev/mins, adopts the carrier of argon stream, according to Al
2O
3: xTi
4+, yMg
2+The stoichiometric ratio of each element passes into triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium in reaction chamber, and wherein, the argon stream amount is 5～15sccm, and
Then pass into oxygen, flow is 10～200sccm; Carrying out chemical vapour deposition, to obtain the luminescent layer chemical formula be Al
2O
3: xTi
4+, yMg
2+, wherein, aluminum oxide is matrix, titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06.
Above-mentioned titanium magnesium codoped aluminum oxide light-emitting film (Al
2O
3: xTi
4+, yMg
2+) electroluminescent spectrum (EL) in, at the 410nm wavelength zone, very strong glow peak is arranged, can be applied in thin-film electroluminescent displays.
[accompanying drawing explanation]
The structural representation of the membrane electro luminescent device that Fig. 1 is an embodiment;
The electroluminescent spectrogram of the titanium magnesium codoped aluminum oxide light-emitting film that Fig. 2 is embodiment 1 preparation;
The XRD figure of the titanium magnesium codoped aluminum oxide light-emitting film that Fig. 3 is embodiment 1 preparation;
Voltage and electric current and the brightness relationship figure of the membrane electro luminescent device that Fig. 4 is embodiment 1 preparation.
[embodiment]
Below in conjunction with the drawings and specific embodiments, titanium magnesium codoped aluminum oxide light-emitting film, its preparation method and membrane electro luminescent device and preparation method thereof are further illustrated.
The titanium magnesium codoped aluminum oxide light-emitting film of one embodiment, its chemical formula is Al
2O
3: xTi
4+, yMg
2+, wherein, aluminum oxide is matrix, titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06.
Preferably, the thickness of titanium magnesium codoped aluminum oxide light-emitting film is 80nm～300nm, and x is that 0.05, y is 0.03.
In this titanium magnesium codoped aluminum oxide light-emitting film, aluminum oxide is matrix, and titanium elements and magnesium elements are active elements.In the electroluminescent spectrum (EL) of this titanium magnesium codoped aluminum oxide light-emitting film, at the 410nm wavelength zone, very strong glow peak is arranged, can be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned titanium magnesium codoped aluminum oxide light-emitting film 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), is 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 used 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 600 ℃～800 ℃ lower thermal treatments 10 minutes～30 minutes.
Step S13, adjusting substrate temperature are 250 ℃～650 ℃, and rotating speed is 50 rev/mins～1000 rev/mins, adopts the carrier of argon stream, according to Al
2O
3: xTi
4+, yMg
2+The stoichiometric ratio of each element passes into triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium in reaction chamber;
In a preferred embodiment, triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium mol ratios are 1: (0.01～0.08): (0～0.06);
In preferred embodiment, triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium mol ratios are 1: 0.05: 0.03,
In a preferred embodiment, substrate temperature is preferably 500 ℃, and the rotating speed of substrate is preferably 300 rev/mins, and the argon stream amount is 5～15sccm;
In more preferred embodiment, the argon stream amount is 10sccm;
Step S14, then pass into oxygen, carrying out chemical vapour deposition, to obtain its chemical formula of titanium magnesium codoped aluminum oxide light-emitting film be Al
2O
3: xTi
4+, yMg
2+, wherein, aluminum oxide is matrix, titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06.
In a preferred embodiment, the oxygen flow amount is 10～200sccm, and x is that 0.05, y is 0.03.
In more preferred embodiment, the oxygen flow amount is 120sccm.
Stop passing into triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium and argon gas after step S15, deposition, continue to pass into oxygen and make the temperature of titanium magnesium codoped aluminum oxide light-emitting film be down to 80 ℃～150 ℃.
In present embodiment, preferred, make the temperature of titanium magnesium codoped aluminum oxide light-emitting film 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 substrate 1, anode 2, luminescent layer 3 and the negative electrode 4 stacked gradually.
Substrate 1 is glass substrate.Anode 2 is for being formed at the tin indium oxide (ITO) on glass substrate.The material of luminescent layer 3 is titanium magnesium codoped aluminum oxide light-emitting film, and the chemical formula of this titanium magnesium codoped aluminum oxide light-emitting film is Al
2O
3: xTi
4+, yMg
2+, wherein, aluminum oxide is matrix, titanium elements and magnesium elements are active elements, 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, 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) on 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; 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, form luminescent layer 3 on anode 2, the material of luminescent layer 3 is titanium magnesium codoped aluminum oxide light-emitting film, and the chemical formula of this titanium magnesium codoped aluminum oxide light-emitting film is Al
2O
3: xTi
4+, yMg
2+, wherein aluminum oxide is matrix, titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06.
In present embodiment, luminescent layer 3 is made by following steps:
At 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 600 ℃～800 ℃ lower thermal treatments 10 minutes～30 minutes.Also can be without this step.
Secondly, regulating substrate temperature is 250 ℃～650 ℃, and rotating speed is 50 rev/mins～1000 rev/mins, adopts the carrier of argon stream, according to Al
2O
3: xTi
4+, yMg
2+The stoichiometric ratio of each element passes into triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium in reaction chamber;
In a preferred embodiment, triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium mol ratios are 1: (0.01～0.08): (0～0.06);
In preferred embodiment, triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium mol ratios are 1: 0.05: 0.03,
In a preferred embodiment, substrate temperature is preferably 500 ℃, and the rotating speed of substrate is preferably 300 rev/mins, and the argon stream amount is 5～15sccm;
In more preferred embodiment, the 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, the oxygen flow amount is 120sccm.
Finally, the deposition after stop passing into triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium and argon gas, continue to pass into oxygen and make the temperature of titanium magnesium codoped aluminum oxide light-emitting film be down to 80 ℃～150 ℃.
In present embodiment, preferred, make the temperature of titanium magnesium codoped aluminum oxide light-emitting film be down to 100 ℃.Can be without this step.
Step S23, form negative electrode 4 on luminescent layer 3.
In present embodiment, the material of negative electrode 4 is silver (Ag), by evaporation, is formed.
It is below specific embodiment.
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.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 4.0 * 10
-3Pa; Then substrate is carried out to 700 ℃ of thermal treatments 20 minutes, then temperature is reduced to 500 ℃.Open rotating machine, the rotating speed of regulating substrate bracket is 300 rev/mins, passes into organic source triethyl aluminum (CH
3CH
2)
3Al, titanium tetraisopropylate TTIP and two luxuriant magnesium (C
5H
5)
2The mol ratio of Mg is 1: 0.05: 0.03, and gas of carrier gas is argon gas, and the argon stream amount is 10sccm.Pass into oxygen, the 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 Al
2O
3: 0.05Ti
4+, 0.03Mg
2+.Last evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula of the titanium magnesium codoped aluminum oxide light-emitting film obtained in the present embodiment is Al
2O
3: 0.05Ti
4+, 0.03Mg
2+, wherein aluminum oxide is matrix, titanium elements and magnesium elements are active elements.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the titanium magnesium codoped aluminum oxide light-emitting film obtained.As seen from Figure 2, in electroluminescence spectrum, at the 410nm wavelength zone, have during very strong glow peak can be applied to thin-film electroluminescent displays.
Refer to Fig. 3, the XRD curve of the titanium magnesium codoped aluminum oxide light-emitting film that Fig. 3 is embodiment 1 preparation, test comparison standard P DF card.As can be seen from Figure 3 all diffraction peaks can find out that all diffraction peaks are all the crystallization phasess of corresponding aluminum oxide, and do not have doped element and other dephasign to occur, illustrate that the product that this preparation method obtains has good crystalline quality.
Refer to Fig. 4, voltage and electric current and the brightness relationship figure of the membrane electro luminescent device that Fig. 4 is embodiment 1 preparation, 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 79cd/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.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 * 10
-3Pa; Then substrate is carried out to 700 ℃ of thermal treatments 10 minutes, then temperature is reduced to 250 ℃.Open rotating machine, the rotating speed of regulating substrate bracket is 50 rev/mins, passes into organic source triethyl aluminum (CH
3CH
2)
3Al, titanium tetraisopropylate TTIP and two luxuriant magnesium (C
5H
5)
2The mol ratio of Mg is 1: 0.08: 0.06, and gas of carrier gas is argon gas, and the argon stream amount is 10sccm.Pass into oxygen, the 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 Al
2O
3: 0.08Ti
4+, 0.06Mg
2+.Last 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.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 * 10
-2Pa; Then substrate is carried out to 700 ℃ of thermal treatments 30 minutes, then temperature is reduced to 650 ℃.Open rotating machine, the rotating speed of regulating substrate bracket is 1000 rev/mins, passes into organic source triethyl aluminum (CH
3CH
2)
3The mol ratio of Al and titanium tetraisopropylate TTIP is 1: 0.01, and gas of carrier gas is argon gas, and the argon stream amount is 10sccm.Pass into oxygen, the 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 Al
2O
3: 0.01Ti
4+.Last 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.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 * 10
-3Pa; Then substrate is carried out to 700 ℃ of thermal treatments 10 minutes, then temperature is reduced to 300 ℃.Open rotating machine, the rotating speed of regulating substrate bracket is 200 rev/mins, passes into organic source triethyl aluminum (CH
3CH
2)
3Al, titanium tetraisopropylate TTIP and two luxuriant magnesium (C
5H
5)
2The mol ratio of Mg is 1: 0.03: 0.02, and gas of carrier gas is argon gas, and the argon stream amount is 20sccm.Pass into oxygen, the oxygen flow amount is 100sccm, 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 Al
2O
3: 0.03Ti
4+, 0.02Mg
2+.Last evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 5
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.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 * 10
-3Pa; Then substrate is carried out to 700 ℃ of thermal treatments 10 minutes, then temperature is reduced to 300 ℃.Open rotating machine, the rotating speed of regulating substrate bracket is 200 rev/mins, passes into organic source triethyl aluminum (CH
3CH
2)
3Al, titanium tetraisopropylate TTIP and two luxuriant magnesium (C
5H
5)
2The mol ratio of Mg is 1: 0.04: 0.04, and gas of carrier gas is argon gas, and the argon stream amount is 20sccm.Pass into oxygen, the oxygen flow amount is 100sccm, 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 Al
2O
3: 0.04Ti
4+, 0.04Mg
2+.Last evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 6
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.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 * 10
-3Pa; Then substrate is carried out to 700 ℃ of thermal treatments 10 minutes, then temperature is reduced to 300 ℃.Open rotating machine, the rotating speed of regulating substrate bracket is 200 rev/mins, passes into organic source triethyl aluminum (CH
3CH
2)
3Al, titanium tetraisopropylate TTIP and two luxuriant magnesium (C
5H
5)
2The mol ratio of Mg is 1: 0.02: 0.01, and gas of carrier gas is argon gas, and the argon stream amount is 20sccm.Pass into oxygen, the oxygen flow amount is 100sccm, 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 Al
2O
3: 0.02Ti
4+, 0.01Mg
2+.Last evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 7
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.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 * 10
-3Pa; Then substrate is carried out to 700 ℃ of thermal treatments 10 minutes, then temperature is reduced to 300 ℃.Open rotating machine, the rotating speed of regulating substrate bracket is 200 rev/mins, passes into organic source triethyl aluminum (CH
3CH
2)
3Al, titanium tetraisopropylate TTIP and two luxuriant magnesium (C
5H
5)
2The mol ratio of Mg is 1: 0.06: 0.04, and gas of carrier gas is argon gas, and the argon stream amount is 20sccm.Pass into oxygen, the oxygen flow amount is 100sccm, 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 Al
2O
3: 0.06Ti
4+, 0.04Mg
2+.Last evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 8
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.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 * 10
-3Pa; Then substrate is carried out to 700 ℃ of thermal treatments 10 minutes, then temperature is reduced to 300 ℃.Open rotating machine, the rotating speed of regulating substrate bracket is 200 rev/mins, passes into organic source triethyl aluminum (CH
3CH
2)
3Al, titanium tetraisopropylate TTIP and two luxuriant magnesium (C
5H
5)
2The mol ratio of Mg is 1: 0.07: 0.05, and gas of carrier gas is argon gas, and the argon stream amount is 20sccm.Pass into oxygen, the oxygen flow amount is 100sccm, 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 Al
2O
3: 0.07Ti
4+, 0.05Mg
2+.Last 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. a titanium magnesium codoped aluminum oxide light-emitting film, is characterized in that, its chemical formula is Al
2O
3: xTi
4+, yMg
2+, wherein, aluminum oxide is matrix, titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06.
2. titanium magnesium codoped aluminum oxide light-emitting film according to claim 1, is characterized in that, the thickness of described titanium magnesium codoped aluminum oxide light-emitting film is 80nm～300nm.
3. the preparation method of a titanium magnesium codoped aluminum oxide light-emitting film, 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 rev/mins～1000 rev/mins, adopts the carrier of argon stream, according to Al
2O
3: xTi
4+, yMg
2+The stoichiometric ratio of each element passes into triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium in reaction chamber; And
Pass into oxygen, carrying out chemical vapour deposition, to obtain chemical formula be Al
2O
3: xTi
4+, yMg
2+Titanium magnesium codoped aluminum oxide light-emitting film, wherein, aluminum oxide is matrix, titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06.
4. the preparation method of titanium magnesium codoped aluminum oxide light-emitting film according to claim 3, is characterized in that, described triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium mol ratios are 1: (0.01～0.08): (0～0.06).
5. the preparation method of titanium magnesium codoped aluminum oxide light-emitting film according to claim 3, is characterized in that, described argon stream amount is 5～15sccm, and described oxygen flow amount is 10～200sccm.
6. the preparation method of titanium magnesium codoped aluminum oxide light-emitting film according to claim 3, is characterized in that, described substrate is packed into after described reaction chamber described substrate 600 ℃～800 ℃ lower thermal treatments 10 minutes～30 minutes.
7. a membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer stacked gradually, it is characterized in that, the material of described luminescent layer is titanium magnesium codoped aluminum oxide light-emitting film, and the chemical formula of this titanium magnesium codoped aluminum oxide light-emitting film is Al
2O
3: xTi
4+, yMg
2+, wherein, aluminum oxide is matrix, titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06.
8. the preparation method of membrane electro luminescent device according to claim 7, is characterized in that, the thickness of described luminescent layer is 80nm～300nm.
9. the preparation method of a membrane electro luminescent device, is characterized in that, comprises the following steps:
Substrate with anode is provided;
Form luminescent layer on described anode, the film of described luminescent layer is titanium magnesium codoped aluminum oxide light-emitting film, and the chemical formula of this titanium magnesium codoped aluminum oxide light-emitting film is Al
2O
3: xTi
4+, yMg
2+, wherein, aluminum oxide is matrix, titanium elements and magnesium elements are active elements, 0.01≤x≤0.08,0≤y≤0.06;
Form negative electrode on described luminescent 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:
By pack into the reaction chamber of chemical vapor depsotition equipment of described substrate, 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 rev/mins～1000 rev/mins, adopts argon stream as carrier, according to Al
2O
3: xTi
4+, yMg
2+The stoichiometric ratio of each element passes into triethyl aluminum, titanium tetraisopropylate and two luxuriant magnesium in reaction chamber, and wherein, the argon stream amount is 5～15sccm, then passes into oxygen, and the oxygen flow amount is 10～200sccm; Deposit film forms luminescent layer on described anode.
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Cited By (1)
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| CN107068399A (en) * | 2017-03-08 | 2017-08-18 | 同济大学 | A kind of high energy storage density solid film capacitor and preparation method thereof |
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| 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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| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107068399A (en) * | 2017-03-08 | 2017-08-18 | 同济大学 | A kind of high energy storage density solid film capacitor and preparation method thereof |
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