CN103421493B - Europium doping sulfo copper aluminate luminescent thin film, preparation method and application thereof - Google Patents
Europium doping sulfo copper aluminate luminescent thin film, preparation method and application thereof Download PDFInfo
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Abstract
A kind of europium doping sulfo copper aluminate luminescent thin film, its chemical formula is CuAl1-xS2:xEu3+, wherein 0.01≤x≤0.08, CuAl1-xS2Being substrate, europium element is active element.In the electroluminescent spectrum (EL) of this europium doping sulfo copper aluminate luminescent thin film, there is very strong glow peak in 610nm wavelength zone, it is possible to be applied in thin-film electroluminescent displays.The present invention also provides for preparation method and the application thereof of this europium doping sulfo copper aluminate luminescent thin film.
Description
[technical field]
The present invention relates to a kind of europium doping sulfo copper aluminate luminescent thin 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 big, Applicable temperature width, operation are simple, has caused and has paid close attention to widely, and quickly grown.At present, studying colored and to panchromatic TFELD, the thin film that exploitation multiband is luminous, is the developing direction of this problem.But, can be applicable to the europium of thin-film electroluminescent displays doping sulfo copper aluminate luminescent thin film, have not yet to see report.
[summary of the invention]
Based on this, it is necessary to provide a kind of and can be applicable to the europium doping sulfo copper aluminate luminescent thin film of membrane electro luminescent device, this europium of its preparation method doping sulfo copper aluminate luminescent thin film electroluminescent device and preparation method thereof.
A kind of europium doping sulfo copper aluminate luminescent thin film, its chemical formula is CuAl1-xS2:xEu3+, wherein CuAl1-xS2Being substrate, europium element is active element, 0.01≤x≤0.08.
In preferred embodiment, the thickness of europium doping sulfo copper aluminate luminescent thin film is 80nm～300nm；
The preparation method of a kind of europium doping sulfo copper aluminate 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；
Regulating substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to CuAl1-xS2:xEu3+Dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium are passed in reative cell by the stoichiometric proportion of each element, and
Then pass to hydrogen sulfide, carry out chemical vapour deposition (CVD) obtain europium doping its chemical formula of sulfo copper aluminate luminescent thin film be CuAl1-xS2:xEu3+, wherein CuAl1-xS2Being substrate, europium element is active element, 0.01≤x≤0.08.
In a preferred embodiment, dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium mol ratio are 1: (0.92～0.99): (0.01～0.08)；
In a more preferred embodiment, dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium mol ratio are 1: 0.95: 0.05,
In a preferred embodiment, argon stream amount is 5～15sccm, and stink damp flow is 10～200sccm.
A kind of membrane electro luminescent device, this membrane electro luminescent device includes the substrate, anode layer, luminescent layer and the cathode layer that stack gradually, the material of described luminescent layer is europium doping sulfo copper aluminate luminescent thin film, and the chemical formula of this europium doping sulfo copper aluminate luminescent thin film is CuAl1-xS2:xEu3+, wherein CuAl1-xS2Being substrate, europium element is active element, 0.01≤x≤0.08.
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 europium doping sulfo copper aluminate luminescent thin film, and the chemical formula of this europium doping sulfo copper aluminate luminescent thin film is CuAl1-xS2:xEu3+, wherein CuAl1-xS2Being substrate, europium element is active element, 0.01≤x≤0.08；
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；
Regulating substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to CuAl1-xS2:xEu3+Dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium are passed in reative cell by the stoichiometric proportion of each element, and wherein, argon stream amount is 5～15sccm, and
Then passing to hydrogen sulfide, flow is 10～200sccm；Carrying out chemical vapour deposition (CVD), to obtain luminescent layer chemical formula be CuAl1-xS2:xEu3+, wherein CuAl1-xS2Being substrate, europium element is active element, 0.01≤x≤0.08.
Above-mentioned europium doping sulfo copper aluminate luminescent thin film (CuAl1-xS2:xEu3+) electroluminescent spectrum (EL) in, have very strong glow peak in 610nm wavelength zone, it is possible to be applied in thin-film electroluminescent displays.
[accompanying drawing explanation]
Fig. 1 is the structural representation of the membrane electro luminescent device of an embodiment；
Fig. 2 is the electroluminescent spectrogram of the europium doping sulfo copper aluminate luminescent thin film of embodiment 1 preparation；
Fig. 3 is the XRD figure of the europium doping sulfo copper aluminate 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]
It is further elucidated with below in conjunction with the drawings and specific embodiments europium adulterated sulfo copper aluminate luminescent thin film, its preparation method and membrane electro luminescent device and preparation method thereof.
The europium doping sulfo copper aluminate luminescent thin film of one embodiment, its chemical formula is CuAl1-xS2:xEu3+, wherein CuAl1-xS2Being substrate, europium element is active element, 0.01≤x≤0.08.
Preferably, the thickness of europium doping sulfo copper aluminate luminescent thin film is 80nm～300nm, x is 0.05.
CuAl in this europium doping sulfo copper aluminate luminescent thin film1-xS2:xEu3+Being substrate, europium element is active element.In the electroluminescent spectrum (EL) of this europium doping sulfo copper aluminate luminescent thin film, there is very strong glow peak in 610nm wavelength zone, it is possible to be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned europium doping sulfo copper aluminate luminescent thin film, comprises the following steps:
Step S11, 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。
In the present embodiment, substrate is indium tin oxide glass (ITO), it is appreciated that in other embodiments, it is also possible to for fluorine doped tin oxide glass (FTO), the zinc oxide (AZO) mixing aluminum or indium-doped zinc oxide (IZO)；Substrate successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, sends into reative cell after nitrogen is air-dry；
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, adjustment substrate temperature are 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to CuAl1-xS2:xEu3+Dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium are passed in reative cell by the stoichiometric proportion of each element；
In a preferred embodiment, dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium mol ratio are 1: (0.92～0.99): (0.01～0.08)；
In a more preferred embodiment, dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium mol ratio are 1: 0.95: 0.05,
In a preferred embodiment, substrate temperature is preferably 500 DEG C, and the rotating speed of substrate is preferably 300 revs/min, and argon stream amount is 5～15sccm；
In more preferred embodiment, argon stream amount is 10sccm；
Step S14, then passing to hydrogen sulfide, carrying out chemical vapour deposition (CVD), to obtain europium doping its chemical formula of sulfo copper aluminate luminescent thin film be CuAl1-xS2:xEu3+, wherein CuAl1-xS2Being substrate, europium element is active element, 0.01≤x≤0.08.
In a preferred embodiment, stink damp flow is 10～200sccm, x is 0.05.
In more preferred embodiment, stink damp flow is 120sccm.
Stop passing into dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium and helium after step S15, deposition, continue to pass into hydrogen sulfide and make the temperature of europium doping sulfo copper aluminate luminescent thin film be down to 80 DEG C～150 DEG C.
In present embodiment, it is preferred that make the temperature of europium doping sulfo copper aluminate luminescent thin film be down to 100 DEG C.
It is appreciated that step S12 and step S15 can omit.
Referring to Fig. 1, the membrane electro luminescent device 100 of an embodiment, this membrane electro luminescent device 100 includes the substrate 1, anode 2, luminescent layer 3 and the negative electrode 4 that stack gradually.
Substrate 1 is glass substrate.Anode 2 is the tin indium oxide (ITO) being formed in glass substrate.The material of luminescent layer 3 is europium doping sulfo copper aluminate luminescent thin film, and the chemical formula of this europium doping sulfo copper aluminate luminescent thin film is CuAl1-xS2:xEu3+, wherein CuAl1-xS2Being substrate, europium element is active element, 0.01≤x≤0.08.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 there is the substrate 1 of anode 2.
In present embodiment, substrate 1 is glass substrate, and anode 2 is the tin indium oxide (ITO) being formed in glass substrate.It is appreciated that in other embodiments, it is also possible to for fluorine doped tin oxide glass (FTO), the zinc oxide (AZO) mixing aluminum or indium-doped zinc oxide (IZO)；There is the substrate 1 priority acetone of anode 2, dehydrated alcohol and deionized water ultrasonic cleaning and carry out oxygen plasma treatment with to it.
Step S22, on anode 2 formed luminescent layer 3, the material of luminescent layer 3 be europium doping sulfo copper aluminate luminescent thin film, this europium doping sulfo copper aluminate luminescent thin film chemical formula be CuAl1-xS2:xEu3+, wherein CuAl1-xS2Being substrate, europium element is active element, 0.01≤x≤0.08.
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 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 without this step.
Secondly, regulating substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, adopts the carrier of argon stream, according to CuAl1-xS2:xEu3+Dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium are passed in reative cell by the stoichiometric proportion of each element；
In a preferred embodiment, dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium mol ratio are 1: (0.92～0.99): (0.01～0.08)；
In a more preferred embodiment, dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium mol ratio are 1: 0.95: 0.05,
In a preferred embodiment, substrate temperature is preferably 500 DEG C, and the rotating speed of substrate is preferably 300 revs/min, and argon stream amount is 5～15sccm；
In more preferred embodiment, argon stream amount is 10sccm；
Then pass to hydrogen sulfide, carry out chemical vapour deposition film on described anode, form luminescent layer.
In preferred embodiment, the flow of hydrogen sulfide is preferably 10～200sccm；
In more preferred embodiment, stink damp flow is 120sccm.
Finally, stop passing into dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium and helium after deposition, continue to pass into hydrogen sulfide and make the temperature of europium doping sulfo copper aluminate luminescent thin film be down to 80 DEG C～150 DEG C.
In present embodiment, it is preferred that make the temperature of europium doping sulfo copper aluminate luminescent thin film be down to 100 DEG C.Can 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 with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, sends into equipment reaction chamber after nitrogen is air-dry.With mechanical pump and molecular pump, the vacuum of cavity 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 regulating substrate bracket is 300 revs/min, passes into organic source dicyclopentadiene copper ((C5H5)2Cu), trimethyl aluminium (TMAl) and dipivaloylmethane europium (Eu (TMHD)3) mol ratio be 1: 0.95: 0.05, gas of carrier gas is argon, and argon stream amount is 10sccm.Passing into hydrogen sulfide, stink damp flow is 120sccm, starts the deposition of thin film.The thickness of thin film deposits to 150nm, closes organic source and carrier gas, continues logical hydrogen sulfide, and temperature drops to less than 100 DEG C, takes out sample CuAl0.95S2:0.05Eu3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
The chemical general formula of the europium doping sulfo copper aluminate luminescent thin film obtained in the present embodiment is CuAl0.95S2:0.05Eu3+, wherein CuAl0.95S2Being substrate, europium element is active element.
Refer to Fig. 2, Fig. 2 and show the electroluminescence spectrum (EL) of the europium doping sulfo copper aluminate luminescent thin 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 610nm wavelength zone.
Refer to the XRD curve of the europium doping sulfo copper aluminate luminescent thin film that Fig. 3, Fig. 3 are embodiment 1 preparation, test comparison standard PDF card.As can be seen from Figure 3 the diffraction maximum in figure is the peak crystallization of thioaluminate copper, it does not have the diffraction maximum of doped chemical and other impurity occur；Illustrate that the product that this preparation method obtains has good crystalline quality
Refer to Fig. 4, Fig. 4 is voltage and electric current and the brightness relationship figure of the membrane electro luminescent device of embodiment 1 preparation, and curve 1 is voltage and electric current density relation curve in figure 4, it can be seen that device starts luminescence from 6V, curve 2 is voltage and brightness relationship curve, and high-high brightness is 83cd/m2, it was shown that device has the good characteristics of luminescence.
Embodiment 2: substrate is ito glass, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, sends into equipment reaction chamber after nitrogen is air-dry.With mechanical pump and molecular pump, the vacuum of cavity 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 regulating substrate bracket is 50 revs/min, passes into organic source dicyclopentadiene copper ((C5H5)2Cu), trimethyl aluminium (TMAl) and dipivaloylmethane europium (Eu (TMHD)3) mol ratio be 1: 0.92: 0.08, gas of carrier gas is argon, and argon stream amount is 10sccm.Passing into hydrogen sulfide, stink damp flow is 10sccm, starts the deposition of thin film.The thickness of thin film deposits to 80nm, closes organic source and carrier gas, continues logical hydrogen sulfide, and temperature drops to less than 100 DEG C, takes out sample CuAl0.92S2:0.08Eu3+.Last one layer of Ag of evaporation 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, sends into equipment reaction chamber after nitrogen is air-dry.With mechanical pump and molecular pump, the vacuum of cavity 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 regulating substrate bracket is 1000 revs/min, passes into organic source dicyclopentadiene copper ((C5H5)2Cu), trimethyl aluminium (TMAl) and dipivaloylmethane europium (Eu (TMHD)3) mol ratio be 1: 0.99: 0.01, gas of carrier gas is argon, and argon stream amount is 10sccm.Passing into hydrogen sulfide, stink damp flow is 200sccm, starts the deposition of thin film.The thickness of thin film deposits to 300nm, closes organic source and carrier gas, continues logical hydrogen sulfide, and temperature drops to less than 100 DEG C, takes out sample CuAl0.99S2:0.01Eu3+.Last one layer of Ag of evaporation 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, sends into equipment reaction chamber after nitrogen is air-dry.With mechanical pump and molecular pump, the vacuum of cavity 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 regulating substrate bracket is 300 revs/min, passes into organic source (CH3)2Ca、(CH3CH2)3The mol ratio of Al and titanium tetraisopropylate is 1: 0.93: 0.07, and gas of carrier gas is argon, and argon stream amount is 10sccm.Passing into hydrogen sulfide, stink damp flow is 120sccm, starts the deposition of thin film.The thickness of thin film deposits to 150nm, closes organic source and carrier gas, continues logical hydrogen sulfide, and temperature drops to less than 100 DEG C, takes out sample CuAl0.93S2:0.07Eu3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment 5: substrate is the ito glass that Nan Bo company buys, successively cleans 5 minutes with toluene, acetone and EtOH Sonicate, then clean with distilled water flushing, sends into equipment reaction chamber after nitrogen is air-dry.With mechanical pump and molecular pump, the vacuum of cavity 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 regulating substrate bracket is 50 revs/min, passes into organic source (CH3)2Ca、(CH3CH2)3The mol ratio of Al and titanium tetraisopropylate is 1: 0.96: 0.04, and gas of carrier gas is argon, and argon stream amount is 10sccm.Passing into hydrogen sulfide, stink damp flow is 10sccm, starts the deposition of thin film.The thickness of thin film deposits to 80nm, closes organic source and carrier gas, continues logical hydrogen sulfide, and temperature drops to less than 100 DEG C, takes out sample CuAl0.96S2:0.04Eu3+.Last one layer of Ag of evaporation on light-emitting film, as negative electrode.
Embodiment described above only have expressed the several embodiments 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, it is also possible to making some deformation and improvement, these broadly fall into protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (5)
1. the preparation method of an europium doping sulfo copper aluminate 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；
Regulating substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, adopts argon stream as carrier, according to CuAl1-xS2: xEu3+Dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium are passed in reative cell by the stoichiometric proportion of each element；And
Passing into hydrogen sulfide, carrying out chemical vapour deposition (CVD), to obtain chemical formula be CuAl1-xS2: xEu3+Europium doping sulfo copper aluminate luminescent thin film, wherein CuAl1-xS2Being substrate, europium element is active element, 0.01≤x≤0.08.
2. the preparation method of europium according to claim 1 doping sulfo copper aluminate luminescent thin film, it is characterized in that, described dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium mol ratio are 1:(0.92～0.99): (0.01～0.08).
3. the preparation method of europium according to claim 1 doping sulfo copper aluminate luminescent thin film, it is characterised in that described argon stream amount is 5～15sccm, and described stink damp flow is 10～200sccm.
4. the preparation method of europium according to claim 1 doping sulfo copper aluminate luminescent thin film, it is characterised in that described substrate is loaded described substrate heat treatment 10 minutes～30 minutes at 600 DEG C～800 DEG C after described reative cell.
5. 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 europium doping sulfo copper aluminate luminescent thin film, and the chemical formula of this europium doping sulfo copper aluminate luminescent thin film is CuAl1-xS2: xEu3+, wherein CuAl1-xS2Being substrate, europium element is active element, 0.01≤x≤0.08；
Forming negative electrode on the light-emitting layer, wherein, 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；
Regulating substrate temperature is 250 DEG C～650 DEG C, and rotating speed is 50 revs/min～1000 revs/min, adopts argon stream as carrier, according to CuAl1-xS2: xEu3+Dicyclopentadiene copper, trimethyl aluminium and dipivaloylmethane europium are passed in reative cell by the stoichiometric proportion of each element, and wherein, argon stream amount is 5～15sccm, then pass to hydrogen sulfide, and stink damp flow is 10～200sccm；Deposition thin film forms luminescent layer on described anode.
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| Local structure of Mn dopants in CuAlS2 and CuGaS2;W. Zalewski等;《phys. stat. sol. (a)》;20080716;第205卷(第10期);2428-2436 * |
| Si Codoped CuAlS2:Mn Red Phosphor for White LEDs;Kazuaki TSUJI等;《J.Light & Vis. Env.》;20081231;第32卷(第2期);135-138 * |
| Ternary compound phosphors for electroluminescent;Noboru Miura;《Proceedings of Asia Display》;20071231;第1卷;483-487 * |
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