CN104681131A - Conducting film, preparation method of conducting film and application - Google Patents

Conducting film, preparation method of conducting film and application Download PDF

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CN104681131A
CN104681131A CN201310634797.6A CN201310634797A CN104681131A CN 104681131 A CN104681131 A CN 104681131A CN 201310634797 A CN201310634797 A CN 201310634797A CN 104681131 A CN104681131 A CN 104681131A
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layer
sputter
substrate
thickness
sputtering
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周明杰
陈吉星
王平
黄辉
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

The invention relates to a conducting film. The conducting film comprises a D2O3 layer, a D conducting layer and a V2O4 layer, which are laminated, wherein the D2O3 layer is made of aluminum oxide, gallium oxide or indium trioxide, and the D conducting layer is made of metal aluminum, metal gallium or metal indium. The D conducting layer and the high-function V2O5 layer are deposited on the surface of the D2O3 layer to prepare a multilayer conducting film, the D2O3 layer is used as a buffer layer and a matching layer, so that the work function of the conducting film is remarkably improved, and the light transmission property is relatively high. The invention also provides a preparation method and an application of the conducting film.

Description

Conductive film, its preparation method and application
Technical field
The present invention relates to photoelectric semiconductor material, particularly relate to conductive film, its preparation method, the substrate using the organic electroluminescence device of this conductive film, its preparation method and organic electroluminescence device.
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, the doped semiconductor of cadmium oxide is Recent study transparent conductive film material the most widely, has higher visible light transmittance rate and low resistivity.But improve the luminous efficiency of device, require that transparent conductive film anode has higher surface work function.And the work function of the zinc oxide of aluminium, gallium and indium doping generally only has 4.3eV, also 4.5 ~ 5.1eV can only be reached after the process such as UV light radiation or ozone, larger energy level difference distance is also had with the HOMO energy level (being typically 5.7 ~ 6.3eV) of general organic luminous layer, cause the increase of carrier injection potential barrier, hinder the raising of luminous efficiency.
Summary of the invention
Based on this, be necessary, for the lower problem of conductive film work function, to provide the higher conductive film of a kind of work function, its preparation method, the substrate using the organic electroluminescence device of this conductive film, its preparation method and organic electroluminescence device.
A kind of conductive film, comprises stacked D 2o 3layer, D conductive layer and V 2o 5layer, wherein, D 2o 3layer is alundum (Al2O3), and gallic oxide or indium sesquioxide, the material of D conductive layer is metallic aluminium, gallium or indium metal.
Described D 2o 3the thickness of layer is 50nm ~ 150nm, and the thickness of described D layer is 10nm ~ 70nm, described V 2o 5the thickness of layer is 1nm ~ 10nm.
A preparation method for conductive film, comprises the following steps:
Metal D and vanadium metal target and substrate are loaded the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, the vacuum degree of vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -5pa, metal D are metallic aluminium, gallium or indium metal;
At described substrate surface sputter D 2o 3layer, D described in sputter 2o 3the technological parameter of layer is: base target spacing is 45mm ~ 95mm, sputtering power is 30W ~ 150W, magnetron sputtering operating pressure 0.2Pa ~ 4Pa, the flow of working gas is 10sccm ~ 35sccm, working gas is argon gas, and passes into reacting gas oxygen, and underlayer temperature is 250 DEG C ~ 750 DEG C, deposition rate is 1 ~ 10nm/s, obtains D 2o 3film substrate is alundum (Al2O3), gallic oxide or indium sesquioxide;
Stop passing into oxygen, at described D 2o 3the surperficial sputter D conductive layer of layer, described in sputter, the technological parameter of D conductive layer is: sputtering rate 0.5nm/s ~ 5nm/s, and sputtering power is the material of 30W ~ 80W, D conductive layer is metallic aluminium, gallium or indium metal;
Then oxygen is entered, at described D conductive layer surface sputter V 2o 5layer, V described in sputter 2o 5the technological parameter of layer is: sputtering rate 0.3nm/s ~ 3nm/s, and sputtering power is 20W ~ 60W,
Peel off described substrate, obtain described stacked D 2o 3layer, D conductive layer and V 2o 5the conductive film of layer.
Described reacting gas oxygen accounts for oxygen and the total mol ratio of argon gas is 1% ~ 15%.
Described D 2o 3the thickness of layer is 50nm ~ 150nm, and the thickness of described D conductive layer is 10nm ~ 70nm, described V 2o 5the thickness of layer is 1nm ~ 10nm.
A substrate for organic electroluminescence device, comprises the substrate, the D that stack gradually 2o 3layer, D conductive layer and V 2o 5layer, wherein, D 2o 3layer is alundum (Al2O3), and gallic oxide or indium sesquioxide, the material of D conductive layer is metallic aluminium, gallium or indium metal.
Described D 2o 3the thickness of layer is 50nm ~ 150nm, and the thickness of described D conductive layer is 10nm ~ 70nm, described V 2o 5the thickness of layer is 1nm ~ 10nm.
A preparation method for the substrate of organic electroluminescence device, comprises the following steps:
Metal D and vanadium metal target and substrate are loaded the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, the vacuum degree of vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -5pa, metal D is metallic aluminium, gallium or indium metal;
At described substrate surface sputter D 2o 3layer, D described in sputter 2o 3the technological parameter of layer is: base target spacing is 45mm ~ 95mm, sputtering power is 30W ~ 150W, magnetron sputtering operating pressure 0.2Pa ~ 4Pa, the flow of working gas is 10sccm ~ 35sccm, working gas is argon gas, and passes into reacting gas oxygen, and underlayer temperature is 250 DEG C ~ 750 DEG C, deposition rate is 1 ~ 10nm/s, obtains D 2o 3film substrate is alundum (Al2O3), gallic oxide or indium sesquioxide;
Stop passing into oxygen, at described D 2o 3the surperficial sputter D conductive layer of layer, described in sputter, the technological parameter of D conductive layer is: sputtering rate 0.5nm/s ~ 5nm/s, and sputtering power is the material of 30W ~ 80W, D conductive layer is metallic aluminium, gallium or indium metal;
Then oxygen is entered, at described D conductive layer surface sputter V 2o 5layer, V described in sputter 2o 5the technological parameter of layer is: sputtering rate 0.3nm/s ~ 3nm/s, sputtering power is 20W ~ 60W.
Described reacting gas oxygen accounts for oxygen and the total mol ratio of argon gas is 1% ~ 15%.
A kind of organic electroluminescence device, comprise the anode, luminescent layer and the negative electrode that stack gradually, described anode comprises stacked D 2o 3layer, D conductive layer and V 2o 5layer, wherein, D 2o 3layer is alundum (Al2O3), and gallic oxide or indium sesquioxide, the material of D conductive layer is metallic aluminium, gallium or indium metal.
Above-mentioned conductive film passes through at D 2o 3the surface deposition D conductive layer of layer and the V of high work content 2o 5layer prepares multilayer conductive film, D 2o 3layer is both as resilient coating and matching layer, the work function of conductive film is obtained improve and there is higher light transmission significantly, conductive film at 300 ~ 900nm wave-length coverage visible light transmissivity 85% ~ 95%, square resistance scope 5 ~ 30 Ω/, surface work function 5.3 ~ 6.2eV; The preparation method of above-mentioned conductive film, 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, reduces the injection barrier of charge carrier, can improve luminous efficiency significantly.
Accompanying drawing explanation
Fig. 1 is the structural representation of the conductive film of an execution mode;
Fig. 2 is the structural representation of the substrate of the organic electroluminescence device of an execution mode;
Fig. 3 is the structural representation of the organic electroluminescence device of an execution mode;
Fig. 4 is the transmitted spectrum spectrogram of conductive film prepared by embodiment 1;
Fig. 5 is the voltage of device embodiments and current density and brightness relationship figure.
Embodiment
Below in conjunction with the drawings and specific embodiments to conductive film, its preparation method, use the substrate of the organic electroluminescence device of this conductive film, its preparation method and organic electroluminescence device to illustrate further.
Refer to Fig. 1, the conductive film 100 of an execution mode comprises stacked D 2o 3layer 10, D conductive layer 20 and V 2o 5layer 30, wherein, D 2o 3layer is alundum (Al2O3), and gallic oxide or indium sesquioxide, the material of D conductive layer is metallic aluminium, gallium or indium metal.
Described D 2o 3the thickness of layer 10 is 50nm ~ 150nm, is preferably 80nm;
The thickness of described D conductive layer 20 is 10nm ~ 70nm, is preferably 30nm;
Described V 2o 5the thickness of layer 30 is 1nm ~ 10nm, is preferably 2nm.
Above-mentioned conductive film 100 passes through D 2o 3the layer surface deposition D conductive layer 20 of 10 and the V of high work content 2o 5layer 30 prepares multilayer conductive film 100, D 2o 3layer 10 is both as resilient coating and matching layer, the work function of conductive film 100 is obtained improve and there is higher light transmission significantly, conductive film at 300 ~ 900nm wave-length coverage visible light transmissivity 85% ~ 95%, square resistance scope 5 ~ 30 Ω/, surface work function 5.3 ~ 6.2eV.
The preparation method of above-mentioned conductive film 100, comprises the following steps:
S110, by D 2o 3target and substrate load the vacuum cavity of magnetic-controlled sputtering coating equipment, and wherein, the vacuum degree of vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -5pa;
Substrate is glass substrate.Preferably, substrate uses acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning before use.
In present embodiment, the vacuum degree of vacuum cavity is preferably 6 × 10 -4pa.
Step S120, at described substrate surface sputter D 2o 3layer 10, D described in sputter 2o 3the technological parameter of layer 10 is: base target spacing is 35mm ~ 90mm, and sputtering power is 60W ~ 160W, magnetron sputtering operating pressure 0.2Pa ~ 4Pa, and the flow of working gas is 10sccm ~ 35sccm, and underlayer temperature is 250 DEG C ~ 750 DEG C, obtains D 2o 3layer 10.
Preferably, base target spacing is 50mm, and sputtering power is 100W, magnetron sputtering operating pressure 1.0Pa, and working gas is argon gas, and the flow of working gas is 20sccm, and underlayer temperature is 250 DEG C ~ 750 DEG C DEG C.
Described D 2o 3the thickness of layer 10 is 50nm ~ 150nm, is preferably 80nm.
Step S130, stopping pass into oxygen, at described D 2o 3layer 10 surperficial sputter D conductive layer 20, described in sputter, the technological parameter of D conductive layer 20 is: sputtering rate 0.5nm/s ~ 5nm/s, and sputtering power is the material of 30W ~ 80W, D conductive layer is metallic aluminium, gallium or indium metal.
The thickness of described D layer 20 is 10nm ~ 70nm;
Step S140, then enter oxygen, at the surperficial sputter V of described D conductive layer 20 2o 5layer 30, V described in sputter 2o 5the technological parameter of layer 30 is: sputtering rate 0.3nm/s ~ 3nm/s, sputtering power is 20W ~ 60W.
Described V 2o 5the thickness of layer 30 is 1nm ~ 10nm.
At the bottom of step S150, peeling liner, obtain conductive film 100.
Refer to Fig. 2, the substrate 200 of the organic electroluminescence device of an execution mode, comprise stacked substrate 201, D 2o 3layer 202, D layer 203 and V 2o 5layer 204.
Substrate 201 is glass substrate.The thickness of substrate 201 is 0.1mm ~ 3.0mm, is preferably 1mm.
Described D 2o 3the thickness of layer 202 is 50nm ~ 150nm, is preferably 80nm;
The thickness of described D layer 203 is 10nm ~ 70nm, is preferably 30nm;
Described V 2o 5the thickness of layer 204 is 1nm ~ 10nm, is preferably 2nm.
The preparation method of the substrate 200 of above-mentioned organic electroluminescence device, comprises the following steps:
S210, metal D and vanadium metal target and substrate are loaded the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, the vacuum degree of vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -5pa, metal D are metallic aluminium, gallium or indium metal.
Substrate is glass substrate.Preferably, substrate uses acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning before use.
In present embodiment, the vacuum degree of vacuum cavity is preferably 6 × 10 -4pa.
Step S220, at described substrate surface sputter D 2o 3layer 202, D described in sputter 2o 3the technological parameter of layer 202 is: base target spacing is 35mm ~ 90mm, and sputtering power is 60W ~ 160W, magnetron sputtering operating pressure 0.2Pa ~ 2Pa, and the flow of working gas is 15sccm ~ 35sccm, and underlayer temperature is 250 DEG C ~ 750 DEG C, obtains D 2o 3layer 202, obtains D 2o 3film substrate is alundum (Al2O3), gallic oxide or indium sesquioxide.
Described D 2o 3the thickness of layer 202 is 50nm ~ 150nm, is preferably 80nm.
Step S203, stopping pass into oxygen, at described D 2o 3layer 10 surperficial sputter D conductive layer 20, described in sputter, the technological parameter of D conductive layer 20 is: sputtering rate 0.5nm/s ~ 5nm/s, and sputtering power is the material of 30W ~ 80W, D conductive layer is metallic aluminium, gallium or indium metal.
Step S204, then enter oxygen, at the surperficial sputter V of described D conductive layer 20 2o 5layer 30, V described in sputter 2o 5the technological parameter of layer 30 is: sputtering rate 0.3nm/s ~ 3nm/s, sputtering power is 20W ~ 60W.
Refer to Fig. 3, the organic electroluminescence device 300 of an execution mode comprises the substrate 301, anode 302, luminescent layer 303 and the negative electrode 304 that stack gradually.Anode 302 is made up of conductive film 100, comprises stacked D 2o 3layer, D conductive layer and V 2o 5layer.Substrate 301 is glass substrate, is appreciated that the difference according to organic electroluminescence device 300 concrete structure, and substrate 301 can omit.The material of luminescent layer 303 is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl Lip river pyridine of a specified duration-9-vinyl)-4H-pyrans (DCJTB), 9,10-bis--β-naphthylene anthracene (AND), two (2-methyl-oxine)-(4-xenol) aluminium (BALQ), 4-(dintrile methene)-2-isopropyl-6-(1,1,7,7-tetramethyl Lip river of a specified duration pyridine-9-vinyl)-4H-pyrans (DCJTI), dimethylquinacridone (DMQA), oxine aluminium (Alq3), two (4,6-difluorophenyl pyridinato-N, C 2) pyridinecarboxylic closes iridium (FIrpic), two (2-methyl-diphenyl [f, h] quinoxaline) (acetylacetone,2,4-pentanediones) close iridium (Ir (MDQ) 2(acac)) or three (2-phenylpyridines) close iridium (Ir (ppy) 3).The material of negative electrode 304 is silver (Ag), gold (Au), aluminium (Al), platinum (Pt) or magnesium silver alloy.
Described D 2o 3the thickness of layer 10 is 50nm ~ 150nm, is preferably 80nm;
The thickness of described D conductive layer 20 is 10nm ~ 70nm, is preferably 30nm;
Described V 2o 5the thickness of layer 30 is 1nm ~ 10nm, is preferably 2nm.
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 5.3 ~ the 6.2eV of conductive film, and gap is less between the HOMO energy level (being typically 5.7 ~ 6.3eV) of general organic luminous layer, reduce the injection barrier of charge carrier, can luminous efficiency be improved.
Be specific embodiment below.
Embodiment 1
Successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.Aluminium target, the distance of vanadium target and substrate is set as 50mm.With mechanical pump and molecular pump, the vacuum degree of cavity is extracted into 6.0 × 10 -4pa, the working gas flow of argon gas is 20sccm, and pressure is adjusted to 1.0Pa, and underlayer temperature is 300 DEG C, and sputtering power is 100W, and on substrate, sputtering obtains Al 2o 3layer, pass into the oxygen that mole percent is 5%, sputtering rate is 3nm/s, and thickness is 80nm, stops passing into oxygen, successively sputter Al layer, and the sputtering rate of sputter Al layer is 3nm/s, and sputtering power is 30W, and thickness is 30nm, then opens oxygen, sputter V 2o 5sputtering rate be 0.5nm/s, sputtering power is 40W, and thickness is 2nm, obtains Al 2o 3-Al-V 2o 5the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 6 Ω/, surface work function tester records surface work function 6.1eV.
Refer to Fig. 4, Figure 4 shows that the transmitted spectrum of the transparent conductive film obtained, use ultraviolet-uisible spectrophotometer test, test wavelength is 300 ~ 900nm.Film reaches 90% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity as seen from Figure 4.
Select Al 2o 3-Al-V 2o 5the transparent conductive film of multilayer as the anode of organic semiconductor device, at sputter luminescent layer Alq above 3, and negative electrode adopts Ag, prepares organic electroluminescence device.
Refer to Fig. 5, Fig. 5 is the voltage of organic electroluminescence device prepared by above-mentioned device embodiments and current density and brightness relationship figure, curve 1 is voltage and current density relation curve in figure 5, device luminescence from 5.5V can be found out, curve 2 is voltage and brightness relationship curve, and high-high brightness is 120cd/m 2, show that device has the good characteristics of luminescence.
Embodiment 2
Successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.Aluminium target, the distance of vanadium target and substrate is set as 60mm.With mechanical pump and molecular pump, the vacuum degree of cavity is extracted into 5.0 × 10 -4pa, the working gas flow of argon gas is 30sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 250 DEG C, and sputtering power is 150W, and on substrate, sputtering obtains Al 2o 3layer, pass into the oxygen that mole percent is 2%, sputtering rate is 1nm/s, and thickness is 150nm, stops passing into oxygen, successively sputter Al layer, and the sputtering rate of sputter Al layer is 0.5nm/s, and sputtering power is 80W, and thickness is 10nm, then opens oxygen, sputter V 2o 5sputtering rate be 0.3nm/s, sputtering power is 60W, and thickness is 1nm, obtains Al 2o 3-Al-V 2o 5the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 25 Ω/, surface work function tester records surface work function 5.9eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 85% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 3
Successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.Aluminium target, the distance of vanadium target and substrate is set as 95mm.With mechanical pump and molecular pump, the vacuum degree of cavity is extracted into 1.0 × 10 -4pa, the working gas flow of argon gas is 25sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 DEG C, and sputtering power is 30W, and on substrate, sputtering obtains Al 2o 3layer, pass into the oxygen that mole percent is 10%, sputtering rate is 10nm/s, and thickness is 50nm, stops passing into oxygen, successively sputter Al layer, and the sputtering rate of sputter Al layer is 5nm/s, and sputtering power is 75W, and thickness is 20nm, then opens oxygen, sputter V 2o 5sputtering rate be 5nm/s, sputtering power is 30W, and thickness is 10nm, obtains Al 2o 3-Al-V 2o 5the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 6 Ω/, surface work function tester records surface work function 6.1eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 90% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 4
Successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.Gallium target, the distance of vanadium target and substrate is set as 80mm.With mechanical pump and molecular pump, the vacuum degree of cavity is extracted into 3.0 × 10 -4pa, the working gas flow of argon gas is 20sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 600 DEG C, and sputtering power is 120W, and on substrate, sputtering obtains Ga 2o 3layer, pass into the oxygen that mole percent is 12%, sputtering rate is 5nm/s, and thickness is 120nm, stops passing into oxygen, successively sputter Ga layer, and the sputtering rate of sputter Ga layer is 0.5nm/s, and sputtering power is 40W, and thickness is 60nm, then opens oxygen, sputter V 2o 5sputtering rate be 2nm/s, sputtering power is 50W, and thickness is 8nm, obtains Ga 2o 3-Ga-V 2o 5the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 10 Ω/, surface work function tester records surface work function 6.5eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 95% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 5
Successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.Gallium target, the distance of vanadium target and substrate is set as 50mm.With mechanical pump and molecular pump, the vacuum degree of cavity is extracted into 2.0 × 10 -4pa, the working gas flow of argon gas is 20sccm, and pressure is adjusted to 1.0Pa, and underlayer temperature is 650 DEG C, and sputtering power is 100W, and on substrate, sputtering obtains Ga 2o 3layer, pass into the oxygen that mole percent is 9%, sputtering rate is 4nm/s, and thickness is 90nm, stops passing into oxygen, successively sputter Ga layer, sputter Ga 2the sputtering rate of layer is 3.5nm/s, and sputtering power is 40W, and thickness is 45nm, then opens oxygen, sputter V 2o 5sputtering rate be 2nm/s, sputtering power is 45W, and thickness is 3nm, obtains Ga 2o 3-Ga-V 2o 5the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 12 Ω/, surface work function tester records surface work function 6.4eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 88% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 6
Successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.Gallium target, the distance of vanadium target and substrate is set as 50mm.With mechanical pump and molecular pump, the vacuum degree of cavity is extracted into 3.0 × 10 -4pa, the working gas flow of argon gas is 25sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 550 DEG C, and sputtering power is 120W, and on substrate, sputtering obtains Ga 2o 3layer, pass into the oxygen that mole percent is 12%, sputtering rate is 6nm/s, and thickness is 90nm, stops passing into oxygen, successively sputter Ga layer, and the sputtering rate of sputter Ga layer is 3nm/s, and sputtering power is 35W, and thickness is 35nm, then opens oxygen, sputter V 2o 5sputtering rate be 0.8nm/s, sputtering power is 45W, and thickness is 3nm, obtains Ga 2o 3-Ga-V 2o 5the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 32 Ω/, surface work function tester records surface work function 6.5eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 91% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 7
Successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.Indium target, the distance of vanadium target and substrate is set as 80mm.With mechanical pump and molecular pump, the vacuum degree of cavity is extracted into 3.0 × 10 -4pa, the working gas flow of argon gas is 20sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 600 DEG C, and sputtering power is 120W, and on substrate, sputtering obtains In 2o 3layer, pass into the oxygen that mole percent is 12%, sputtering rate is 5nm/s, and thickness is 120nm, stops passing into oxygen, successively sputter In layer, and the sputtering rate of sputter In layer is 0.5nm/s, and sputtering power is 40W, and thickness is 60nm, then opens oxygen, sputter V 2o 5sputtering rate be 2nm/s, sputtering power is 50W, and thickness is 8nm, obtains In 2o 3-In-V 2o 5the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 10 Ω/, surface work function tester records surface work function 6.5eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 95% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 8
Successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.Indium target, the distance of vanadium target and substrate is set as 50mm.With mechanical pump and molecular pump, the vacuum degree of cavity is extracted into 2.0 × 10 -4pa, the working gas flow of argon gas is 20sccm, and pressure is adjusted to 1.0Pa, and underlayer temperature is 650 DEG C, and sputtering power is 100W, and on substrate, sputtering obtains In 2o 3layer, pass into the oxygen that mole percent is 9%, sputtering rate is 4nm/s, and thickness is 90nm, stops passing into oxygen, successively sputter In layer, and the sputtering rate of sputter In layer is 3.5nm/s, and sputtering power is 40W, and thickness is 45nm, then opens oxygen, sputter V 2o 5sputtering rate be 2nm/s, sputtering power is 45W, and thickness is 3nm, obtains In 2o 3-In-V 2o 5the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 12 Ω/, surface work function tester records surface work function 6.4eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 88% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 9
Successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning glass substrate, put into vacuum cavity.Indium target, the distance of vanadium target and substrate is set as 50mm.With mechanical pump and molecular pump, the vacuum degree of cavity is extracted into 3.0 × 10 -4pa, the working gas flow of argon gas is 25sccm, and pressure is adjusted to 3.0Pa, and underlayer temperature is 550 DEG C, and sputtering power is 120W, and on substrate, sputtering obtains In 2o 3layer, pass into the oxygen that mole percent is 12%, sputtering rate is 6nm/s, and thickness is 90nm, stops passing into oxygen, successively sputter In layer, and the sputtering rate of sputter In layer is 3nm/s, and sputtering power is 35W, and thickness is 35nm, then opens oxygen, sputter V 2o 5sputtering rate be 0.8nm/s, sputtering power is 45W, and thickness is 3nm, obtains In 2o 3-In-V 2o 5the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 32 Ω/, surface work function tester records surface work function 6.5eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 91% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
The above embodiment only have expressed several execution mode 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 range 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 D 2o 3layer, D conductive layer and V 2o 5layer, wherein, D 2o 3layer is alundum (Al2O3), and gallic oxide or indium sesquioxide, the material of D conductive layer is metallic aluminium, gallium or indium metal.
2. conductive film according to claim 1, is characterized in that, described D 2o 3the thickness of layer is 50nm ~ 150nm, and the thickness of described D layer is 10nm ~ 70nm, described V 2o 5the thickness of layer is 1nm ~ 10nm.
3. a preparation method for conductive film, is characterized in that, comprises the following steps:
Metal D and vanadium metal target and substrate are loaded the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, the vacuum degree of vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -5pa, metal D are metallic aluminium, gallium or indium metal;
At described substrate surface sputter D 2o 3layer, D described in sputter 2o 3the technological parameter of layer is: base target spacing is 45mm ~ 95mm, sputtering power is 30W ~ 150W, magnetron sputtering operating pressure 0.2Pa ~ 4Pa, the flow of working gas is 10sccm ~ 35sccm, working gas is argon gas, and passes into reacting gas oxygen, and underlayer temperature is 250 DEG C ~ 750 DEG C, deposition rate is 1 ~ 10nm/s, obtains D 2o 3film substrate is alundum (Al2O3), gallic oxide or indium sesquioxide;
Stop passing into oxygen, at described D 2o 3the surperficial sputter D conductive layer of layer, described in sputter, the technological parameter of D conductive layer is: sputtering rate 0.5nm/s ~ 5nm/s, and sputtering power is the material of 30W ~ 80W, D conductive layer is metallic aluminium, gallium or indium metal;
Then oxygen is entered, at described D conductive layer surface sputter V 2o 5layer, V described in sputter 2o 5the technological parameter of layer is: sputtering rate 0.3nm/s ~ 3nm/s, and sputtering power is 20W ~ 60W,
Peel off described substrate, obtain described stacked D 2o 3layer, D conductive layer and V 2o 5the conductive film of layer.
4. the preparation method of conductive film according to claim 3, is characterized in that, described reacting gas oxygen accounts for oxygen and the total mol ratio of argon gas is 1% ~ 15%.
5. the preparation method of conductive film according to claim 3, is characterized in that, described D 2o 3the thickness of layer is 50nm ~ 150nm, and the thickness of described D conductive layer is 10nm ~ 70nm, described V 2o 5the thickness of layer is 1nm ~ 10nm.
6. a substrate for organic electroluminescence device, is characterized in that, comprises the substrate, the D that stack gradually 2o 3layer, D conductive layer and V 2o 5layer, wherein, D 2o 3layer is alundum (Al2O3), and gallic oxide or indium sesquioxide, the material of D conductive layer is metallic aluminium, gallium or indium metal.
7. the substrate of organic electroluminescence device according to claim 6, is characterized in that, described D 2o 3the thickness of layer is 50nm ~ 150nm, and the thickness of described D conductive layer is 10nm ~ 70nm, described V 2o 5the thickness of layer is 1nm ~ 10nm.
8. a preparation method for the substrate of organic electroluminescence device, is characterized in that, comprises the following steps:
Metal D and vanadium metal target and substrate are loaded the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, the vacuum degree of vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -5pa, metal D are metallic aluminium, gallium or indium metal;
At described substrate surface sputter D 2o 3layer, D described in sputter 2o 3the technological parameter of layer is: base target spacing is 45mm ~ 95mm, sputtering power is 30W ~ 150W, magnetron sputtering operating pressure 0.2Pa ~ 4Pa, the flow of working gas is 10sccm ~ 35sccm, working gas is argon gas, and passes into reacting gas oxygen, and underlayer temperature is 250 DEG C ~ 750 DEG C, deposition rate is 1 ~ 10nm/s, obtains D 2o 3film substrate is alundum (Al2O3), gallic oxide or indium sesquioxide;
Stop passing into oxygen, at described D 2o 3the surperficial sputter D conductive layer of layer, described in sputter, the technological parameter of D conductive layer is: sputtering rate 0.5nm/s ~ 5nm/s, and sputtering power is the material of 30W ~ 80W, D conductive layer is metallic aluminium, gallium or indium metal;
Then oxygen is entered, at described D conductive layer surface sputter V 2o 5layer, V described in sputter 2o 5the technological parameter of layer is: sputtering rate 0.3nm/s ~ 3nm/s, sputtering power is 20W ~ 60W.
9. the preparation method of the substrate of organic electroluminescence device according to claim 8, is characterized in that, described reacting gas oxygen accounts for oxygen and the total mol ratio of argon gas is 1% ~ 15%.
10. an organic electroluminescence device, comprise the anode, luminescent layer and the negative electrode that stack gradually, it is characterized in that, described anode comprises stacked D 2o 3layer, D conductive layer and V 2o 5layer, wherein, D 2o 3layer is alundum (Al2O3), and gallic oxide or indium sesquioxide, the material of D conductive layer is metallic aluminium, gallium or indium metal.
CN201310634797.6A 2013-11-30 2013-11-30 Conducting film, preparation method of conducting film and application Pending CN104681131A (en)

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