CN103289690B - Praseodymium doped titanate luminescent film, preparation method and application thereof - Google Patents
Praseodymium doped titanate luminescent film, preparation method and application thereof Download PDFInfo
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- CN103289690B CN103289690B CN201210047881.3A CN201210047881A CN103289690B CN 103289690 B CN103289690 B CN 103289690B CN 201210047881 A CN201210047881 A CN 201210047881A CN 103289690 B CN103289690 B CN 103289690B
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Abstract
A kind of praseodymium doped titanate luminescent film, its chemical expression is MeTi
1-xo
3: xPr
3+, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg, Ca, Sr or Ba.In the electroluminescent spectrum (EL) of this praseodymium doped titanate luminescent film, there is very strong glow peak in 611nm wavelength zone, can be applied in thin-film electroluminescent displays.The present invention also provides preparation method and the application thereof of this praseodymium doped titanate luminescent film.
Description
[technical field]
The present invention relates to a kind of praseodymium doped titanate luminescent film, its preparation method, membrane electro luminescent device and preparation method thereof.
[background technology]
Thin-film electroluminescent displays (TFELD), due to its active illuminating, total solids, the advantage such as shock-resistant, reaction is fast, visual angle is large, Applicable temperature is wide, operation is simple, has caused and paid close attention to widely, and development rapidly.At present, research colour and extremely panchromatic TFELD, the material of exploitation multiband luminescence is the developing direction of this problem.But, can be applicable to the praseodymium doped titanate luminescent 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 can be applicable to membrane electro luminescent device praseodymium doped titanate luminescent film, its preparation method, use this praseodymium doped titanate luminescent film electroluminescent device and preparation method thereof.
A kind of praseodymium doped titanate luminescent film, the chemical expression of this praseodymium doped titanate luminescent film is MeTi
1-xo
3: xPr
3+, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg, Ca, Sr or Ba;
In more preferred embodiment, the thickness of described praseodymium doped titanate luminescent film is 80nm ~ 300nm.
A preparation method for praseodymium doped titanate luminescent film, comprises the following steps:
Substrate is loaded the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10
-2pa ~ 1.0 × 10
-3pa;
Regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, under the carrier of argon stream, according to MeTi
1-xo
3: xPr
3+the stoichiometric ratio of each element is by (DPM)
2me, titanium tetraisopropylate and Pr (DPM)
3pass in reaction chamber; And
Then pass into oxygen, carrying out chemical vapour deposition, to obtain its chemical expression of praseodymium doped titanate luminescent film be MeTi
1-xo
3: xPr
3+, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg, Ca, Sr or Ba.
In a preferred embodiment, (DPM)
2me, titanium tetraisopropylate and Pr (DPM)
3mol ratio is 1: (0.92 ~ 0.99): (0.01 ~ 0.08).
In a preferred embodiment, described argon stream amount is 5 ~ 15sccm, and described oxygen flow amount is 10 ~ 200sccm.
In a preferred embodiment, described substrate is loaded the thermal treatment 10 minutes ~ 30 minutes at 600 DEG C ~ 800 DEG C of described substrate after described reaction chamber.
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 praseodymium doped titanate luminescent film, and the chemical expression of this praseodymium doped titanate luminescent film is MeTi
1-xo
3: xPr
3+, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg, Ca, Sr or Ba.
In a preferred embodiment, the thickness of described luminescent layer is 80nm ~ 300nm.
A preparation method for membrane electro luminescent device, comprises the following steps:
The substrate with anode is provided;
Described anode forms luminescent layer, and the material of described luminescent layer is praseodymium doped titanate luminescent film, and the chemical expression of this praseodymium doped titanate luminescent film is MeTi
1-xo
3: xPr
3+, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg, Ca, Sr or Ba; And
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 the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10
-2pa ~ 1.0 × 10
-3pa;
Regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, under the carrier of argon stream, according to MeTi
1-xo
3: xPr
3+the stoichiometric ratio of each element is by (DPM)
2me, titanium tetraisopropylate and Pr (DPM)
3pass in reaction chamber, argon stream amount is 5 ~ 15sccm; And
Then pass into oxygen, flow is 10 ~ 200sccm; Carry out chemical vapour deposition film and form luminescent layer on described anode.
Above-mentioned praseodymium doped titanate luminescent film (MeTi
1-xo
3: xPr
3+) in the electroluminescent spectrum (EL) of light-emitting film made, have very strong glow peak in 611nm 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 praseodymium doped titanate luminescent film prepared by embodiment 1;
Fig. 3 is the XRD figure of praseodymium doped titanate luminescent film prepared by embodiment 1.
[embodiment]
Below in conjunction with the drawings and specific embodiments, praseodymium doped titanate luminescent film, its preparation method, membrane electro luminescent device and preparation method thereof are illustrated further.
The praseodymium doped titanate luminescent film of one embodiment, the chemical general formula of this praseodymium doped titanate luminescent film is MeTi
1-xo
3: xPr
3+, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg, Ca, Sr or Ba.
The thickness of praseodymium doped titanate luminescent film is 80nm ~ 300nm
Preferably, x is 0.05, and thickness is 150nm.
MeAl in this praseodymium doped titanate luminescent film
2-xo
4be matrix, Ti element is active element.In the electroluminescent spectrum (EL) of this praseodymium doped titanate luminescent film, there is very strong glow peak in 611nm wavelength zone, can be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned praseodymium doped titanate luminescent film, comprises the following steps:
Step S11, substrate is loaded the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10
-2pa ~ 1.0 × 10
-3pa.
In present embodiment, substrate is indium tin oxide glass (ITO), be appreciated that in other embodiments, can be also fluorine doped tin oxide glass (FTO), mix the zinc oxide (AZO) of aluminium or mix the zinc oxide (IZO) of indium; Substrate priority toluene, acetone and EtOH Sonicate clean 5 minutes, then clean with distilled water flushing, the air-dry rear feeding reaction chamber of nitrogen; Preferably, the vacuum tightness of reaction chamber is 4.0 × 10
-3pa.
Step S12, by substrate thermal treatment 10 minutes ~ 30 minutes at 600 DEG C ~ 800 DEG C.
Step S13, adjustment substrate temperature are 250 DEG C ~ 650 DEG C, and rotating speed is 50 revs/min ~ 1000 revs/min, under the carrier of argon stream, according to MeTi
1-xo
3: xPr
3+the stoichiometric ratio of each element is by dipivaloylmethane hydrochlorate { (DPM)
2me}, titanium tetraisopropylate and Pr (DPM)
3pass in reaction chamber, argon stream amount is 5 ~ 15sccm.
In this step, preferably, (DPM)
2me, titanium tetraisopropylate and Pr (DPM)
3mol ratio is 1: (0.92 ~ 0.99): (0.01 ~ 0.08), and argon stream amount is 5 ~ 15sccm;
Preferred, (DPM)
2me, titanium tetraisopropylate and Pr (DPM)
3mol ratio is 1: 0.95: 0.05, and described argon stream amount is 10sccm;
Step S23, then pass into oxygen, flow is 10 ~ 200sccm; Carrying out chemical vapour deposition, to obtain its chemical expression of praseodymium doped titanate luminescent film be MeTi
1-xo
3: xPr
3+, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg, Ca, Sr or Ba.
In this step, preferably, oxygen flow is 10 ~ 200sccm;
In this step, preferred, oxygen flow is 120sccm, x is 0.05.
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 praseodymium doped titanate luminescent film, and the chemical expression of this praseodymium doped titanate luminescent film is MeTi
1-xo
3: xPr
3+, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg, Ca, Sr or Ba.The material of negative electrode 4 is silver (Ag).
The preparation method of above-mentioned membrane electro luminescent device, comprises the following steps:
Step S31, provide the substrate 1 with anode 2.
In present embodiment, substrate 1 is glass substrate, anode 2 is for being formed at the tin indium oxide (ITO) in glass substrate, in other embodiments, anode 2 can be also fluorine doped tin oxide (FTO), mixes the zinc oxide (AZO) of aluminium or mix the zinc oxide (IZO) of indium.Have the substrate 1 priority toluene of anode 2, acetone and EtOH Sonicate and clean 5 minutes, then clean with distilled water flushing, nitrogen is air-dry.
Step S32, on anode 2, form luminescent layer 3, the material of luminescent layer 3 is praseodymium doped titanate luminescent film, and the chemical expression of this praseodymium doped titanate luminescent film is MeTi
1-xo
3: xPr
3+, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg, Ca, Sr or Ba.
In present embodiment, luminescent layer 3 is obtained by following steps:
First, substrate is loaded the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10
-2pa ~ 1.0 × 10
-3pa;
Secondly, regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, under the carrier of argon stream, according to MeTi
1-xo
3: xPr
3+the stoichiometric ratio of each element is by (DPM)
2me, titanium tetraisopropylate and Pr (DPM)
3pass in reaction chamber, argon stream amount is 5 ~ 15sccm;
Preferably, (DPM)
2me, titanium tetraisopropylate and Pr (DPM)
3mol ratio is 1: (0.92 ~ 0.99): (0.01 ~ 0.08);
Preferred, (DPM)
2me, titanium tetraisopropylate and Pr (DPM)
3mol ratio is 1: 0.95: 0.05, and described argon stream amount is 10sccm;
Finally, then pass into oxygen, flow is 10 ~ 200sccm; Carrying out chemical vapour deposition, to obtain its chemical expression of praseodymium doped titanate luminescent film be MeTi
1-xo
3: xPr
3+, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg, Ca, Sr or Ba.
In this step, preferably, oxygen flow is 120sccm, x is 0.05.
Step S33, on luminescent layer 3, form negative electrode 4.
In present embodiment, the material of negative electrode 4 is silver (Ag), is formed by evaporation.
Be specific embodiment below.
Embodiment 1
Substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 4.0 × 10
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, passes into organic source (DPM)
2mg, titanium tetraisopropylate and Pr (DPM)
3mol ratio be 1: 0.95: 0.05, gas of carrier gas is argon gas, and 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, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out sample MgTi
0.95o
3: 0.05Pr
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
The chemical general formula of the praseodymium doped titanate luminescent film obtained in the present embodiment is MgTi
0.95o
3: 0.05Pr
3+, wherein MgTi
0.95o
3be matrix, Pr element is active element.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the praseodymium doped titanate luminescent film obtained.As seen from Figure 2, in electroluminescence spectrum, there is very strong glow peak can be applied in thin-film electroluminescent displays in 611nm wavelength zone.
Refer to Fig. 3, Fig. 3 is the XRD curve of praseodymium doped titanate luminescent film prepared by embodiment 1, test comparison standard P DF card.As can be seen from Figure 3 reference standard PDF card, is the peak crystallization of titanate, 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.
Embodiment 2
Substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, passes into organic source (DPM)
2mg, titanium tetraisopropylate and Pr (DPM)
3mol ratio be 1: 0.92: 0.08, gas of carrier gas is argon gas, and 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, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out sample MgTi
0.92o
3: 0.08Pr
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 3
Substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, passes into organic source (DPM)
2mg, titanium tetraisopropylate and Pr (DPM)
3mol ratio be 1: 0.99: 0.01, gas of carrier gas is argon gas, and 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, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out sample MgTi
0.99o
3: 0.01Pr
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 4: substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 4.0 × 10
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, passes into organic source (DPM)
2ca, titanium tetraisopropylate and Pr (DPM)
3mol ratio be 1: 0.95: 0.05, gas of carrier gas is argon gas, and 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, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out sample CaTi
0.95o
3: 0.05Pr
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 5: substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, passes into organic source (DPM)
2ca, titanium tetraisopropylate and Pr (DPM)
3mol ratio be 1: 0.92: 0.08, gas of carrier gas is argon gas, and 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, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out sample CaTi
092o
3: 0.08Pr
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 6: substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, passes into organic source (DPM)
2ca, titanium tetraisopropylate and Pr (DPM)
3mol ratio be 1: 0.99: 0.01, gas of carrier gas is argon gas, and 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, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out sample CaTi
0.99o
3: 0.01Pr
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 7: substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 4.0 × 10
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, passes into organic source (DPM)
2sr, titanium tetraisopropylate and Pr (DPM)
3mol ratio be 1: 0.95: 0.05, gas of carrier gas is argon gas, and 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, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out sample SrTi
0.95o
3: 0.05Pr
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 8: substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, passes into organic source (DPM)
2sr, titanium tetraisopropylate and Pr (DPM)
3mol ratio be 1: 0.92: 0.08, gas of carrier gas is argon gas, and 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, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out sample SrTi
0.92o
3: 0.08Pr
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 9: substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, passes into organic source (DPM)
2sr, titanium tetraisopropylate and Pr (DPM)
3mol ratio be 1: 0.99: 0.01, gas of carrier gas is argon gas, and 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, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out sample SrTi
0.99o
3: 0.01PrW.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 10: substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 4.0 × 10
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 20 minutes, then temperature reduces to 500 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 300 revs/min, passes into organic source (DPM)
2ba, titanium tetraisopropylate and Pr (DPM)
3mol ratio be 1: 0.95: 0.05, gas of carrier gas is argon gas, and 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, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out sample BaTi
0.95o
3: 0.05Pr
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 11: substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-3pa; Then substrate is carried out 700 DEG C of thermal treatments 10 minutes, then temperature reduces to 250 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 50 revs/min, passes into organic source (DPM)
2ba, titanium tetraisopropylate and Pr (DPM)
3mol ratio be 1: 0.92: 0.08, gas of carrier gas is argon gas, and 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, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out sample BaTi
0.92o
3: 0.08Pr
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
Embodiment 12: substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, the air-dry rear feeding equipment reaction chamber of nitrogen.With mechanical pump and molecular pump, the vacuum tightness of cavity is evacuated to 1.0 × 10
-2pa; Then substrate is carried out 700 DEG C of thermal treatments 30 minutes, then temperature reduces to 650 DEG C.Open rotating machine, the rotating speed regulating substrate bracket is 1000 revs/min, passes into organic source (DPM)
2ba, titanium tetraisopropylate and Pr (DPM)
3mol ratio be 1: 0.99: 0.01, gas of carrier gas is argon gas, and 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, and continue logical oxygen, temperature drops to less than 100 DEG C, takes out sample BaTi
0.99o
3: 0.01Pr
3+.Finally evaporation one deck Ag on light-emitting film, as negative electrode.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a praseodymium doped titanate luminescent film, is characterized in that: its chemical expression is MeTi
1-xo
3: xPr
3+, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg.
2. praseodymium doped titanate luminescent film according to claim 1, is characterized in that, the thickness of described praseodymium doped titanate luminescent film is 80nm ~ 300nm.
3. a preparation method for praseodymium doped titanate luminescent film, is characterized in that, comprises the following steps:
Substrate is loaded the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10
-2pa ~ 1.0 × 10
-3pa;
Regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, under the carrier of argon stream, according to MeTi
1-xo
3: xPr
3+the stoichiometric ratio of each element is by (DPM)
2me, titanium tetraisopropylate and Pr (DPM)
3pass in reaction chamber, wherein, DPM is dipivaloylmethane acid; And
Pass into oxygen, carrying out chemical vapour deposition, to obtain chemical expression be MeTi
1-xo
3: xPr
3+praseodymium doped titanate luminescent film, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg.
4. the preparation method of praseodymium doped titanate luminescent film according to claim 3, is characterized in that, described (DPM)
2me, titanium tetraisopropylate and Pr (DPM)
3mol ratio be 1:(0.92 ~ 0.99): (0.01 ~ 0.08).
5. the preparation method of praseodymium doped titanate luminescent 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 praseodymium doped titanate luminescent film according to claim 3, is characterized in that, is loaded the thermal treatment 10 minutes ~ 30 minutes at 600 DEG C ~ 800 DEG C of described substrate by described substrate after described reaction chamber.
7. a membrane electro luminescent device, comprises the substrate, anode layer, luminescent layer and the cathode layer that stack gradually, it is characterized in that, described luminescent layer is praseodymium doped titanate luminescent film, and the chemical expression of this praseodymium doped titanate luminescent film is MeTi
1-xo
3: xPr
3+, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg.
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. a preparation method for membrane electro luminescent device, is characterized in that, comprises the following steps:
The substrate with anode is provided;
Described anode forms luminescent layer, and described luminescent layer is praseodymium doped titanate luminescent film, and the chemical expression of this praseodymium doped titanate luminescent film is MeTi
1-xo
3: xPr
3+, wherein MeTi
1-xo
3be matrix, Pr element is active element, 0.01≤x≤0.08, and Me is Mg; And
Form negative electrode on the light-emitting layer.
10. the preparation method of membrane electro luminescent device according to claim 9, is characterized in that, the preparation of described luminescent layer comprises the following steps:
Substrate is loaded the reaction chamber of chemical vapor depsotition equipment, and the vacuum tightness of reaction chamber is set to 1.0 × 10
-2pa ~ 1.0 × 10
-3pa;
Regulate substrate temperature to be 250 DEG C ~ 650 DEG C, rotating speed is 50 revs/min ~ 1000 revs/min, under the carrier of argon stream, according to MeTi
1-xo
3: xPr
3+the stoichiometric ratio of each element is by (DPM)
2me, titanium tetraisopropylate and Pr (DPM)
3pass in reaction chamber, wherein, DPM is dipivaloylmethane acid, and argon stream amount is 5 ~ 15sccm; And
Pass into oxygen, oxygen flow amount is 10 ~ 200sccm; Carry out chemical vapour deposition film and form luminescent layer on described anode.
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