CN103660418A - Conducting film, and preparation method and application thereof - Google Patents
Conducting film, and preparation method and application thereof Download PDFInfo
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- CN103660418A CN103660418A CN201210350689.1A CN201210350689A CN103660418A CN 103660418 A CN103660418 A CN 103660418A CN 201210350689 A CN201210350689 A CN 201210350689A CN 103660418 A CN103660418 A CN 103660418A
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Abstract
The invention provides a conducting film which comprises a ZITO (zinc-indium-tin oxide) layer and a MoO3 layer which are laminated, wherein the ZITO layer is a film layer containing zinc oxide, indium oxide and tin oxide, and has higher light transmittance and lower resistance; and compared with the common transparent conducting film, the nanowire assembly prepared from the film enhances the light emitting efficiency of the organic electroluminescent device. The double-layer conducting film prepared by depositing the molybdenum trioxide layer on the surface of the ZITO layer has higher surface work function, can lower the trigger voltage of the device and can enhance the luminescence efficiency. The invention also provides a preparation method and application of the conducting film.
Description
Technical field
The present invention relates to photoelectric semiconductor material, particularly relate to conductive film, its preparation method, use substrate, its preparation method and the organic electroluminescence device of the organic electroluminescence device of this conductive film.
Background technology
Conductive film electrode is the basic component of organic electroluminescence device (OLED), and the quality of its performance directly affects the luminous efficiency of whole device.Wherein, transparent conductive film is optical clear performance and electric conductivity to be compounded in to the photoelectric material of one, because it has excellent photoelectric characteristic, become study hotspot and advanced subject in recent years, can be widely used in solar cell, LED, TFT, the screen display fields such as LCD and touch-screen.The raising requiring along with device performance, also improves requiring for the performance of the nesa coating as device anode.For the needs of device light extraction efficiency, a lot of research institutions are all managing to insert scattering layer between anode and substrate.
High performance device, also requires anode to have higher surface work function, and the energy level of itself and other functional layer is matched, and reduces potential barrier, improves Carrier Injection Efficiency, finally reaches high electrical efficiency.
Summary of the invention
Based on this, be necessary conductive film, its preparation method that provides a kind of work function higher, the substrate that uses the organic electroluminescence device of this conductive film, its preparation method and organic electroluminescence device.
A conductive film, comprises stacked ZITO layer and MoO
3layer, wherein, ZITO layer is zinc oxide, the thin layer of indium oxide and doped sno_2.
A preparation method for conductive film, comprises the following steps:
By ZITO target, MoO
3target and substrate pack the vacuum cavity of pulsed laser deposition equipment into, and wherein, the vacuum of vacuum cavity is 1.0 * 10
-3pa ~ 1.0 * 10
-5pa, ZITO target is zinc oxide, indium oxide and doped sno_2 target;
At described substrate surface deposition ZITO layer, the technological parameter that deposits described ZITO layer is: base target spacing is 45mm ~ 95mm, and pulsed laser power is 80W ~ 300W, operating pressure 3Pa ~ 30Pa, the flow of working gas is 10sccm ~ 40sccm, and underlayer temperature is 250 ℃ ~ 750 ℃;
At described ZITO layer surface deposition MoO
3layer, the technological parameter that deposits described ZITO layer is: base target spacing is 45mm ~ 95mm, pulsed laser power is 80W ~ 300W, operating pressure 3Pa ~ 30Pa, the flow of working gas is 10sccm ~ 40sccm, underlayer temperature is 250 ℃ ~ 750 ℃; And
Peel off described substrate, obtain described conductive film.
In an embodiment, the thickness of described ZITO layer is 80nm ~ 150nm, described MoO therein
3the thickness of layer is 3nm ~ 15nm.
In an embodiment, described ZITO target is obtained by following steps therein: according to each component mol ratio, be (0.1 ~ 10): (70 ~ 98): (0.5 ~ 20) by ZnO, In
2o3 and SnO
2powder mixes, and the powder mixing sintering at 900 ℃ ~ 1300 ℃ is made to target.
Therein in an embodiment, described MoO
3target is obtained by following steps: by MoO
3powder sintering at 700 ℃ ~ 1100 ℃ is made target.
A substrate for organic electroluminescence device, comprises the substrate, ZITO layer and the MoO that stack gradually
3layer, wherein, ZITO layer is zinc oxide, the thin layer of indium oxide and doped sno_2.
A preparation method for the substrate of organic electroluminescence device, comprises the following steps:
By ZITO target, MoO
3target and substrate pack the vacuum cavity of pulsed laser deposition equipment into, and wherein, the vacuum of vacuum cavity is 1.0 * 10
-3pa ~ 1.0 * 10
-5pa, ZITO target is zinc oxide, indium oxide and doped sno_2 target;
At described substrate surface deposition ZITO layer, the technological parameter that deposits described ZITO layer is: base target spacing is 45mm ~ 95mm, and pulsed laser power is 80W ~ 300W, operating pressure 3Pa ~ 30Pa, the flow of working gas is 10sccm ~ 40sccm, and underlayer temperature is 250 ℃ ~ 750 ℃; And
At described ZITO layer surface deposition MoO
3layer, deposits described MoO
3the technological parameter of layer is: base target spacing is 45mm ~ 95mm, and pulsed laser power is 80W ~ 300W, operating pressure 3Pa ~ 30Pa, and the flow of working gas is 10sccm ~ 40sccm, underlayer temperature is 250 ℃ ~ 750 ℃.
In an embodiment, described ZITO target is obtained by following steps therein: according to each component mol ratio, be (0.1 ~ 10): (70 ~ 98): (0.5 ~ 20) by ZnO, In
2o3 and SnO
2powder mixes, and the powder mixing sintering at 900 ℃ ~ 1300 ℃ is made to target.
Therein in an embodiment, described MoO
3target is obtained by following steps: by MoO
3powder sintering at 700 ℃ ~ 1100 ℃ is made target.
An organic electroluminescence device, comprises the anode, luminescent layer and the negative electrode that stack gradually, and described anode comprises stacked substrate, ZITO layer and MoO
3layer, wherein, ZITO layer is zinc oxide, the thin layer of indium oxide and doped sno_2.
Above-mentioned conductive film is prepared double-deck conductive film by the surface deposition Molybdenum Oxide Thin Films by Sol-Gel at ZITO layer, conductive film is made the set of nano wire, there is higher surface work function, can guarantee high printing opacity again, the light extraction efficiency that is conducive to device improves, conductive film is at the long scope visible light transmissivity 85% ~ 91% of 470 ~ 790nm, square resistance scope 10 ~ 73 Ω/, surface work function 4.8 ~ 5.5eV; The preparation method of above-mentioned conductive film, uses pulsed laser deposition equipment to get final product continuous production ZITO layer and MoO
3layer, technique is comparatively simple; Use this conductive film as the anode of organic electroluminescence device, between the surface work function of conductive film and the HOMO energy level of general organic luminous layer, gap is less, has reduced the injection barrier of carrier, can improve significantly luminous efficiency.
Accompanying drawing explanation
Fig. 1 is the structural representation of the conductive film of an embodiment;
Fig. 2 is the structural representation of substrate of the organic electroluminescence device of an embodiment;
Fig. 3 is the structural representation of the organic electroluminescence device of an embodiment;
Fig. 4 is the transmitted light spectrogram of the conductive film of embodiment 1 preparation;
Fig. 5 is the electron-microscope scanning figure of the conductive film of embodiment 1 preparation;
Fig. 6 is the electroluminescent device of embodiment 1 preparation and brightness and the voltage curve of comparative example comparison.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, conductive film, its preparation method, the substrate that uses the organic electroluminescence device of this conductive film, its preparation method and organic electroluminescence device are further illustrated.
Refer to Fig. 1, the conductive film 100 of an embodiment comprises stacked ZITO layer 30 and MoO
3layer 10, wherein, ZITO layer 30 is zinc oxide, the thin layer of indium oxide and doped sno_2.
The thickness of ZITO layer 30 is 80nm ~ 150nm, is preferably 120nm.
MoO
3the thickness of layer 10 is 3nm～15nm, is preferably 5nm.
Above-mentioned conductive film 100 is by the surface deposition MoO at ZITO layer 30
3the double-deck conductive film of layer 10 film preparation, the double-deck conductive film of preparation can keep good electric conductivity like this, make again the work function of conductive film 100 obtain significant raising, conductive film 100 is at 470 ~ 790nm wave-length coverage visible light transmissivity 85% ~ 91%, square resistance scope 10 Ω/ ~ 73 Ω/, surface work function 4.8eV ~ 5.5eV.
The preparation method of above-mentioned conductive film 100, comprises the following steps:
S110, by ZITO target, MoO
3target and substrate pack the vacuum cavity of pulsed laser deposition equipment into, and wherein, the vacuum of vacuum cavity is 1.0 * 10
-3pa ~ 1.0 * 10
-5pa, ZITO target is zinc oxide, indium oxide and doped sno_2 target.
In present embodiment, ZITO target is obtained by following steps: according to each component mol ratio, be (0.1 ~ 10): (70 ~ 98): (0.5 ~ 20) by ZnO, In
2o3 and SnO
2powder mixes, and the powder mixing sintering at 900 ℃ ~ 1300 ℃ is made to target.
MoO
3target is obtained by following steps: MoO
3target is obtained by following steps: by MoO
3powder sintering at 700 ℃ ~ 1100 ℃ is made target.
Substrate is glass substrate.Preferably, substrate is used acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning before use.
In present embodiment, the vacuum of vacuum cavity is preferably 5 * 10
-4pa.
Step S120, at substrate surface deposition ZITO layer 30, the technological parameter that deposits described ZITO layer 30 is: base target spacing is 45mm ~ 95mm, and pulsed laser power is 80W ~ 300W, operating pressure 3Pa ~ 30Pa, the flow of working gas is 10sccm ~ 40sccm, and underlayer temperature is 250 ℃ ~ 750 ℃.
Preferably, base target spacing is 60mm, and pulsed laser power is 150W, operating pressure 10Pa, and working gas is argon gas, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃.
The thickness of the ZITO layer 30 forming is 80nm～150nm, is preferably 120nm.
Step S130, at described ZITO layer 30 surface deposition MoO
3layer 10, deposits described MoO
3the technological parameter of layer 10 is: base target spacing is 45mm ~ 95mm, and pulsed laser power is 80W ~ 300W, operating pressure 3Pa ~ 30Pa, and the flow of working gas is 10sccm ~ 40sccm, underlayer temperature is 250 ℃ ~ 750 ℃.
Preferably, base target spacing is 60mm, and pulsed laser power is 150W, operating pressure 10Pa, and working gas is argon gas, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃.
The MoO forming
3the thickness of layer 10 is 3nm ~ 15nm, is preferably 5nm.
At the bottom of step S140, peeling liner, obtain conductive film 100.
The preparation method of above-mentioned conductive film, only uses pulsed laser deposition equipment to get final product continuous production ZITO layer 30 and MoO
3layer 10, technique is comparatively simple.
Refer to Fig. 2, the substrate 200 of the organic electroluminescence device of an embodiment, comprises stacked substrate 201, ZITO layer 202 and MoO
3layer 203, wherein, ZITO layer 202 is zinc oxide, the thin layer of indium oxide and doped sno_2.
The thickness of ZITO layer 202 is 80nm ~ 150nm, is preferably 120nm.
MoO
3the thickness of layer 203 is 3nm ~ 15nm, is preferably 5nm.
The substrate 200 of above-mentioned organic electroluminescence device is by the surface deposition MoO at ZITO layer 202
3 layer 203, can keep good electric conductivity, makes again the work function of the substrate 200 of organic electroluminescence device obtain significant raising.
The preparation method of the substrate 200 of above-mentioned organic electroluminescence device, comprises the following steps:
S210, by ZITO target, MoO
3target and substrate pack the vacuum cavity of pulsed laser deposition equipment into, and wherein, the vacuum of vacuum cavity is 1.0 * 10
-3pa ~ 1.0 * 10
-5pa, ZITO target is zinc oxide, indium oxide and doped sno_2 target.
In present embodiment, ZITO target is obtained by following steps: according to each component mol ratio, be (0.1 ~ 10): (70 ~ 98): (0.5 ~ 20) by ZnO, In
2o3 and SnO
2powder mixes, and the powder mixing sintering at 900 ℃ ~ 1300 ℃ is made to target.
MoO
3target is obtained by following steps: MoO
3target is obtained by following steps: by MoO
3powder sintering at 700 ℃ ~ 1100 ℃ is made target.
Substrate is glass substrate.Preferably, substrate is used acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning before use.
In present embodiment, the vacuum of vacuum cavity is preferably 5 * 10
-4pa.
Step S220, at substrate surface sputter ZITO layer 202, the technological parameter of sputter ZITO layer 202 is: base target spacing is 45mm ~ 95mm, and pulsed laser power is 80W ~ 300W, operating pressure 3Pa ~ 30Pa, the flow of working gas is 10sccm ~ 40sccm, and underlayer temperature is 250 ℃ ~ 750 ℃.
Preferably, base target spacing is 60mm, and pulsed laser power is 150W, operating pressure 10Pa, and working gas is argon gas, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃.
The thickness of the ZITO layer 202 forming is 80nm ~ 150nm, is preferably 12nm.
Step S230, at the surperficial sputter MoO of ZITO layer 202
3 layer 203, sputter MoO
3the technological parameter of layer 203 is: base target spacing is 45mm ~ 95mm, and pulsed laser power is 80W ~ 300W, operating pressure 3Pa ~ 30Pa, and the flow of working gas is 10sccm ~ 40sccm, underlayer temperature is 250 ℃ ~ 750 ℃.
Preferably, base target spacing is 60mm, and pulsed laser power is 150W, operating pressure 10Pa, and working gas is argon gas, and the flow of working gas is 20sccm, and underlayer temperature is 500 ℃.
The MoO forming
3the thickness of layer 203 is 3nm ~ 15nm, is preferably 5nm.
The preparation method of the substrate 200 of above-mentioned organic electroluminescence device, uses pulsed laser deposition equipment can on substrate 201, prepare continuously ZITO layer 202 and MoO
3layer 203, technique is comparatively simple.
Refer to Fig. 3, the organic electroluminescence device 300 of an embodiment comprises substrate 301, anode 302, luminescent layer 303 and the negative electrode 304 stacking gradually.
The thickness of ZITO layer is 80nm ~ 150nm, is preferably 120nm.MoO
3the thickness of layer is 3nm ~ 15nm, is preferably 5nm.
Be appreciated that above-mentioned organic electroluminescence device 300 also can arrange other functional layers according to user demand.
Above-mentioned organic electroluminescence device 300, use conductive film 100 as the anode of organic electroluminescence device, surface work function 4.8 ~ the 5.5eV of conductive film, and between the HOMO energy level (being typically 5.7～6.3eV) of general organic luminous layer, gap is less, reduce the injection barrier of carrier, can improve luminous efficiency.
Be specific embodiment below.
Embodiment 1
Select the ZnO of 0.05mol, the In of 0.9mol
2the SnO of O3 and 0.05mol
2after even mixing, at 1250 ℃, sintering diameter into is 50mm, the ZITO ceramic target that thickness is 2mm, MoO
3powder is under 1000 ℃ of conditions, and making diameter is 50mm, the MoO that thickness is 2mm
3ceramic target, and target is packed in the cavity of pulsed laser deposition chamber.Then, successively use acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.The distance of target and substrate is set as to 60mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 5.0 * 10
-4pa, the working gas flow of argon gas is 20sccm, and pressure is adjusted to 10Pa, and underlayer temperature is 500 ℃, and pulsed laser power is 150W.Priority sputter ZITO and MoO
3target, deposit respectively the film of 120nm and 5nm, on substrate, obtain ZITO-MoO
3double-deck transparent conductive film is as the anode of organic semiconductor device, and luminescent layer adopts Alq
3, negative electrode adopts Ag.
Test result: adopt four point probe resistance meter to record square resistance scope 10 Ω/, surface work function tester records surface work function 5.5eV.
Refer to Fig. 4, Figure 4 shows that the transmitted spectrum of the transparent conductive film obtaining, use ultraviolet-uisible spectrophotometer test, test wavelength is 300 ~ 800nm.Film mean transmissivity in visible ray 470nm ~ 790nm wave-length coverage has reached 88% as seen from Figure 4.
Refer to Fig. 5, Fig. 5 is the electron-microscope scanning figure of the conductive film of embodiment 1 preparation, and ZITO columnar nanometer line vertical-growth, on substrate, forms film as seen from the figure.
Refer to Fig. 6, Fig. 6 is the electroluminescent device of embodiment 1 preparation and brightness and the voltage curve of comparative example comparison, curve 1 is membrane electro luminescent device voltage and the brightness relationship curve of embodiment 1 preparation as seen from Figure 6, curve 2 is membrane electro luminescent device voltage and brightness relationship curves prepared by comparative example, can find out: can find out that nanometer wire sample reduces from 4.0 to 3.5V the starting resistor of device, brightness improves.
Comparative example
By the In of the ZnO of 0.05mol, 0.9mol
2the SnO of O3 and 0.05mol
2powder is after even mixing, at 1250 ℃, sinter into and be of a size of diameter 50, thickness is that the ceramic target of 2mm is the shape of cake, and target is packed in vacuum cavity, by transparent glass substrate, successively use toluene, acetone and ethanol ultrasonic cleaning 5 minutes, then clean with distilled water flushing, and use and it is carried out to nitrogen dry up, put into vacuum cavity.The distance of target and substrate is set as to 60mm, with mechanical pump and molecular pump, the vacuum of cavity is evacuated to 5.0 * 10
-4pa; Adopt oxygen as working air current, working gas flow is 15sccm, and pressure is adjusted to 1.0Pa, and underlayer temperature is 500 ℃, pulsed laser energy 150W, successively sputter ZITO and MoO
3target, deposit respectively the film of 120nm and 5nm, on substrate, obtain ZITO-MoO
3double-deck transparent conductive film is as the anode of organic semiconductor device, and luminescent layer adopts Alq
3, negative electrode adopts Ag.
The method is to adopt laser ablation target, make the aluminium oxide in target, the ablated particle that becomes atom or ion cluster of gallium oxide and the materials such as zinc oxide, in the process that particle deposits in substrate, by passing into a large amount of inert gases, make particle passivation, on substrate, disperse nucleation, then at each nucleating point vertical-growth, the pillared nano wire of shape.Amount and pressure that the thickness of nano wire and distance between centers of tracks can pass into inert gas by adjusting control.In theory, pass into inert gas pressure large, the nano wire obtaining is thinner, and distance between centers of tracks is larger.
Comparative example is the conventional technique of preparation normal transparent conducting film, passes into oxygen and can make ablation particle activation out, and on substrate, nucleation directly laterally generates film forming.
Select the ZnO of 0.001mol, the In of 0.949mol
2the SnO of O3 and 0.05mol
2after even mixing, at 900 ℃, sintering diameter into is 50mm, the ZITO ceramic target that thickness is 2mm, MoO
3powder is under 700 ℃ of conditions, and making diameter is 50mm, the MoO that thickness is 2mm
3ceramic target, and target is packed in the cavity of pulsed laser deposition chamber.Then, successively use acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.The distance of target and substrate is set as to 45mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 1.0 * 10
-3pa, the working gas flow of argon gas is 10sccm, and pressure is adjusted to 3Pa, and underlayer temperature is 250 ℃, and pulsed laser power is 300W.Priority sputter ZITO and MoO
3target, deposit respectively the film of 80nm and 15nm, obtain ZITO-MoO
3double-deck transparent conductive film is as the anode of organic semiconductor device, and luminescent layer adopts Alq
3, negative electrode adopts Ag.
Test result: adopt four point probe resistance meter to record square resistance scope 15 Ω/, surface work function 5.2eV, the test of use ultraviolet-uisible spectrophotometer, test wavelength is that 300 ~ 800nm film mean transmissivity in visible ray 470nm ~ 790nm wave-length coverage has reached 90%.
Select the ZnO of 0.1mol, the In of 0.895mol
2the SnO of O3 and 0.005mol
2after even mixing, at 1300 ℃, sintering diameter into is 50mm, the ZITO ceramic target that thickness is 2mm, MoO
3powder is under 1100 ℃ of conditions, and making diameter is 50mm, the MoO that thickness is 2mm
3ceramic target, and target is packed in the cavity of pulsed laser deposition chamber.Then, successively use acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.The distance of target and substrate is set as to 95mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 1.0 * 10
-5pa, the working gas flow of argon gas is 40sccm, and pressure is adjusted to 30Pa, and underlayer temperature is 750 ℃, and pulsed laser power is 80W.Priority sputter ZITO and MoO
3target, deposit respectively the film of 150nm and 3nm, on substrate, obtain ZITO-MoO
3double-deck transparent conductive film is as the anode of organic semiconductor device, and luminescent layer adopts Alq
3, negative electrode adopts Ag.
Test result: adopt four point probe resistance meter to record square resistance scope 33 Ω/, surface work function 4.9e V, the test of use ultraviolet-uisible spectrophotometer, test wavelength is that 300 ~ 800nm film mean transmissivity in visible ray 470nm ~ 790nm wave-length coverage has reached 90%.
Embodiment 4
Select the ZnO of 0.1mol, the In of 0.7mol
2the SnO of O3 and 0.2mol
2after even mixing, at 1000 ℃, sintering diameter into is 50mm, the ZITO ceramic target that thickness is 2mm, MoO
3powder is under 700 ℃ of conditions, and making diameter is 50mm, the MoO that thickness is 2mm
3ceramic target, and target is packed in the cavity of pulsed laser deposition chamber.Then, successively use acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.The distance of target and substrate is set as to 60mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 5.0 * 10
-4pa, the working gas flow of argon gas is 20sccm, and pressure is adjusted to 10Pa, and underlayer temperature is 500 ℃, and pulsed laser power is 150W.Successively sputter MoO
3with the target of ZITO, deposit respectively the film of 90nm and 8nm, obtain ZITO-MoO
3double-deck transparent conductive film is as the anode of organic semiconductor device, and luminescent layer adopts Alq
3, negative electrode adopts Ag.
Test result: adopt four point probe resistance meter to record square resistance scope 73 Ω/, surface work function 4.8eV, the test of use ultraviolet-uisible spectrophotometer, test wavelength is that 300 ~ 800nm film mean transmissivity in visible ray 470nm ~ 790nm wave-length coverage has reached 91%.
Select the ZnO of 0.02mol, the In of 0.92mol
2the SnO of O3 and 0.06mol
2after even mixing, at 1000 ℃, sintering diameter into is 50mm, the ZITO ceramic target that thickness is 2mm, MoO
3powder is under 800 ℃ of conditions, and making diameter is 50mm, the MoO that thickness is 2mm
3ceramic target, and target is packed in the cavity of pulsed laser deposition chamber.Then, successively use acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.The distance of target and substrate is set as to 48mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 7.0 * 10
-4pa, the working gas flow of argon gas is 10sccm, and pressure is adjusted to 8Pa, and underlayer temperature is 350 ℃, and pulsed laser power is 250W.Priority sputter ZITO and MoO
3target, deposit respectively the film of 100nm and 14nm, obtain ZITO-MoO
3double-deck transparent conductive film is as the anode of organic semiconductor device, and luminescent layer adopts Alq
3, negative electrode adopts Ag.
Test result: adopt four point probe resistance meter to record square resistance scope 19 Ω/, surface work function 5.1eV, the test of use ultraviolet-uisible spectrophotometer, test wavelength is that 300 ~ 800nm film mean transmissivity in visible ray 470nm ~ 790nm wave-length coverage has reached 91%.
Embodiment 6
Select the ZnO of 0.03mol, the In of 0.88mol
2the SnO of O3 and 0.09mol
2after even mixing, at 1100 ℃, sintering diameter into is 50mm, the ZITO ceramic target that thickness is 2mm, MoO
3powder is under 850 ℃ of conditions, and making diameter is 50mm, the MoO that thickness is 2mm
3ceramic target, and target is packed in the cavity of pulsed laser deposition chamber.Then, successively use acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.The distance of target and substrate is set as to 52mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 9.0 * 10
-4pa, the working gas flow of argon gas is 10sccm, and pressure is adjusted to 8Pa, and underlayer temperature is 380 ℃, and pulsed laser power is 180W.Priority sputter ZITO and MoO
3target, deposit respectively the film of 110nm and 13nm, obtain ZITO-MoO
3double-deck transparent conductive film is as the anode of organic semiconductor device, and luminescent layer adopts Alq
3, negative electrode adopts Ag.
Test result: adopt four point probe resistance meter to record square resistance scope 22 Ω/, surface work function 4.9eV, the test of use ultraviolet-uisible spectrophotometer, test wavelength is that 300 ~ 800nm film mean transmissivity in visible ray 470nm ~ 790nm wave-length coverage has reached 89%.
Select the ZnO of 0.04mol, the In of 0.9mol
2the SnO of O3 and 0.06mol
2after even mixing, at 1150 ℃, sintering diameter into is 50mm, the ZITO ceramic target that thickness is 2mm, MoO
3powder is under 950 ℃ of conditions, and making diameter is 50mm, the MoO that thickness is 2mm
3ceramic target, and target is packed in the cavity of pulsed laser deposition chamber.Then, successively use acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.The distance of target and substrate is set as to 48mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 6.5 * 10
-4pa, the working gas flow of argon gas is 10sccm, and pressure is adjusted to 6Pa, and underlayer temperature is 380 ℃, and pulsed laser power is 120W.Priority sputter ZITO and MoO
3target, deposit respectively the film of 95nm and 9nm, obtain ZITO-MoO
3double-deck transparent conductive film is as the anode of organic semiconductor device, and luminescent layer adopts Alq
3, negative electrode adopts Ag.
Test result: adopt four point probe resistance meter to record square resistance scope 20 Ω/, surface work function 5.0eV, the test of use ultraviolet-uisible spectrophotometer, test wavelength is that 300 ~ 800nm film mean transmissivity in visible ray 470nm ~ 790nm wave-length coverage has reached 92%.
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 conductive film, is characterized in that, comprises stacked ZITO layer and MoO
3layer, wherein, ZITO layer is zinc oxide, the thin layer of indium oxide and doped sno_2.
2. a preparation method for conductive film, is characterized in that, comprises the following steps:
By ZITO target, MoO
3target and substrate pack the vacuum cavity of pulsed laser deposition equipment into, and wherein, the vacuum of vacuum cavity is 1.0 * 10
-3pa ~ 1.0 * 10
-5pa, ZITO target is zinc oxide, indium oxide and doped sno_2 target;
At described substrate surface deposition ZITO layer, the technological parameter that deposits described ZITO layer is: base target spacing is 45mm ~ 95mm, and pulsed laser power is 80W ~ 300W, operating pressure 3Pa ~ 30Pa, the flow of inert working gas is 10sccm ~ 40sccm, and underlayer temperature is 250 ℃ ~ 750 ℃;
At described ZITO layer surface deposition MoO
3layer, deposits described MoO
3the technological parameter of layer is: base target spacing is 45mm ~ 95mm, and pulsed laser power is 80W ~ 300W, operating pressure 3Pa ~ 30Pa, and the flow of working gas is 10sccm ~ 40sccm, underlayer temperature is 250 ℃ ~ 750 ℃;
Peel off described substrate, obtain described conductive film.
3. the preparation method of conductive film according to claim 2, is characterized in that, the thickness of described ZITO layer is 80nm ~ 150nm, described MoO
3the thickness of layer is 3nm ~ 15nm.
4. the preparation method of conductive film according to claim 2, is characterized in that, described ZITO target is obtained by following steps: according to each component mol ratio, be (0.1 ~ 10): (70 ~ 98): (0.5 ~ 20) by ZnO, In
2o3 and SnO
2powder mixes, and the powder mixing sintering at 900 ℃ ~ 1300 ℃ is made to target.
5. the preparation method of conductive film according to claim 2, is characterized in that, described MoO
3target is obtained by following steps: by MoO
3powder sintering at 700 ℃ ~ 1100 ℃ is made target.
6. a substrate for organic electroluminescence device, is characterized in that, comprises the substrate, ZITO layer and the MoO that stack gradually
3layer, wherein, ZITO layer is zinc oxide, the thin layer of indium oxide and doped sno_2.
7. a preparation method for the substrate of organic electroluminescence device, is characterized in that, comprises the following steps:
By ZITO target, MoO
3target and substrate pack the vacuum cavity of pulsed laser deposition equipment into, and wherein, the vacuum of vacuum cavity is 1.0 * 10
-3pa ~ 1.0 * 10
-5pa, ZITO target is zinc oxide, indium oxide and doped sno_2 target;
At described substrate surface deposition ZITO layer, the technological parameter that deposits described ZITO layer is: base target spacing is 45mm ~ 95mm, and pulsed laser power is 80W ~ 300W, operating pressure 3Pa ~ 30Pa, the flow of working gas is 10sccm ~ 40sccm, and underlayer temperature is 250 ℃ ~ 750 ℃; And
At described ZITO layer surface deposition MoO
3layer, deposits described MoO
3the technological parameter of layer is: base target spacing is 45mm ~ 95mm, and pulsed laser power is 80W ~ 300W, operating pressure 3Pa ~ 30Pa, and the flow of working gas is 10sccm ~ 40sccm, underlayer temperature is 250 ℃ ~ 750 ℃.
8. the preparation method of the substrate of organic electroluminescence device according to claim 7, is characterized in that, described ZITO target is obtained by following steps: according to each component mol ratio, be (0.1 ~ 10): (70 ~ 98): (0.5 ~ 20) by ZnO, In
2o3 and SnO
2powder mixes, and the powder mixing sintering at 900 ℃ ~ 1300 ℃ is made to target.
9. the preparation method of the substrate of organic electroluminescence device according to claim 7, is characterized in that, described MoO
3target is obtained by following steps: by MoO
3powder sintering at 700 ℃ ~ 1100 ℃ is made target.
10. an organic electroluminescence device, comprises the anode, luminescent layer and the negative electrode that stack gradually, it is characterized in that, described anode comprises substrate, ZITO layer and the MoO stacking gradually
3layer, wherein, ZITO layer is zinc oxide, the thin layer of indium oxide and doped sno_2.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109830545A (en) * | 2019-02-14 | 2019-05-31 | 中国科学院半导体研究所 | A kind of aluminum-doped zinc oxide films surface modifying material, preparation method and battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109830545A (en) * | 2019-02-14 | 2019-05-31 | 中国科学院半导体研究所 | A kind of aluminum-doped zinc oxide films surface modifying material, preparation method and battery |
| CN109830545B (en) * | 2019-02-14 | 2021-10-15 | 中国科学院半导体研究所 | Aluminum-doped zinc oxide film surface modification material, preparation method and battery |
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