CN104339746A - Conductive film, and preparation method and application thereof - Google Patents

Conductive film, and preparation method and application thereof Download PDF

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Publication number
CN104339746A
CN104339746A CN201310337079.2A CN201310337079A CN104339746A CN 104339746 A CN104339746 A CN 104339746A CN 201310337079 A CN201310337079 A CN 201310337079A CN 104339746 A CN104339746 A CN 104339746A
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layer
mgo
evaporation
substrate
conductive layer
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周明杰
陈吉星
王平
冯小明
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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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Priority to CN201310337079.2A priority Critical patent/CN104339746A/en
Publication of CN104339746A publication Critical patent/CN104339746A/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/081—Oxides of aluminium, magnesium or beryllium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

The invention relates to a conductive film comprising a MgO layer, a conductive layer and a Co3O4 layer which are laminated. The material of the conductive layer is one selected from gold, silver, copper and platinum. According to the invention, the conductive layer and the high-work-function Co3O4 layer are deposited on the surface of the MgO layer, such that the multi-layer conductive film is obtained. The MgO layer serves as a buffering layer and a matching layer, such that work function of the conductive film is substantially improved, and the film has relatively high translucency. The invention also provides a preparation method and an application of the conductive 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 MgO layer, conductive layer and Co 3o 4layer, wherein the material of conductive layer is selected from gold, silver, the one in copper and platinum.
The thickness of described MgO layer is 40nm ~ 160nm, and the thickness of described conductive layer is 5nm ~ 40nm, described Co 3o 4the thickness of layer is 1nm ~ 10nm.
A preparation method for conductive film, comprises the following steps:
MgO target and substrate are loaded the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, the vacuum of vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -5pa;
At described substrate surface sputter MgO layer, described in sputter, the technological parameter of MgO layer is: base target spacing is 45mm ~ 85mm, sputtering power is 80W ~ 200W, magnetron sputtering operating pressure 0.2Pa ~ 2Pa, the flow of working gas is 15sccm ~ 35sccm, underlayer temperature is 200 DEG C ~ 700 DEG C, obtains MgO film substrate;
Then MgO film substrate is put into evaporated device cavity, the vacuum regulating vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -6pa,
At described MgO layer surface evaporation conductive layer, the technological parameter of conductive layer described in evaporation is: evaporation rate 0.5 ~ 3nm/s, evaporation time 10 ~ 80s, and the material of described conductive layer is selected from gold, silver, the one in copper and platinum;
At described conductive layer surface evaporation Co 3o 4layer, Co described in evaporation 3o 4the technological parameter of layer is: evaporation rate 0.2 ~ 2nm/s, evaporation time 5 ~ 50s, and
Peel off described substrate, obtain described conductive film.
Described MgO target is obtained by following steps: sintered at 800 DEG C ~ 1400 DEG C by MgO powder and make target.
The thickness of described MgO layer is 40nm ~ 160nm, and the thickness of described conductive layer is 5nm ~ 40nm, described Co 3o 4the thickness of layer is 1nm ~ 10nm.
A substrate for organic electroluminescence device, comprises the substrate stacked gradually, stacked MgO layer, conductive layer and Co 3o 4layer, wherein the material of conductive layer is selected from gold, silver, the one in copper and platinum.
The thickness of described MgO layer is 40nm ~ 160nm, and the thickness of described conductive layer is 5nm ~ 40nm, described Co 3o 4the thickness of layer is 1nm ~ 10nm.
A preparation method for the substrate of organic electroluminescence device, comprises the following steps:
MgO target and substrate are loaded the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, the vacuum of vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -5pa;
At described substrate surface sputter MgO layer, described in sputter, the technological parameter of MgO layer is: base target spacing is 45mm ~ 85mm, sputtering power is 80W ~ 200W, magnetron sputtering operating pressure 0.2Pa ~ 2Pa, the flow of working gas is 15sccm ~ 35sccm, underlayer temperature is 200 DEG C ~ 700 DEG C, obtains MgO film substrate;
Then MgO film substrate is put into evaporated device cavity, the vacuum regulating vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -6pa,
At described MgO layer surface evaporation conductive layer, the technological parameter of conductive layer described in evaporation is: evaporation rate 0.5 ~ 3nm/s, evaporation time 10 ~ 80s, and the material of described conductive layer is selected from gold, silver, the one in copper and platinum;
At described conductive layer surface evaporation Co 3o 4layer, Co described in evaporation 3o 4the technological parameter of layer is: evaporation rate 0.2 ~ 2nm/s, evaporation time 5 ~ 50s.
Described MgO target is obtained by following steps: sintered at 800 DEG C ~ 1400 DEG C by MgO powder and make target.
A kind of organic electroluminescence device, comprise the anode, luminescent layer and the negative electrode that stack gradually, it is characterized in that, described anode comprises stacked MgO layer, conductive layer and Co 3o 4layer, wherein the material of conductive layer is selected from gold, silver, the one in copper and platinum.
Above-mentioned conductive film passes through at the surface deposition conductive layer of MgO layer and the Co of high work content 3o 4layer prepares multilayer conductive film, MgO layer is both as cushion and matching layer, the work function of conductive film is obtained improve and there is higher light transmission significantly, conductive film is at 300 ~ 900nm wave-length coverage visible light transmissivity 85% ~ 95%, square resistance scope 2 Ω/ ~ 15 Ω/, surface work function 5.6eV ~ 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 carrier, can improve luminous efficiency significantly.
Accompanying drawing explanation
Fig. 1 is the structural representation of the conductive film of an embodiment;
Fig. 2 is the structural representation of the 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 spectrum spectrogram of conductive film prepared by embodiment 1;
Fig. 5 is the voltage of device embodiments and electric current and brightness relationship figure.
Detailed description of the invention
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 embodiment comprises stacked MgO layer 10, conductive layer 20 and Co 3o 4layer 30, wherein, the material of conductive layer is selected from gold, silver, the one in copper and platinum.
The thickness of described MgO layer 10 is 40nm ~ 160nm, is preferably 80nm;
The thickness of described conductive layer 20 is 5nm ~ 40nm, is preferably 22nm;
Described Co 3o 4the thickness of layer 30 is 1nm ~ 10nm, is preferably 3.5nm.
Above-mentioned conductive film 100 is by the surface deposition conductive layer 20 of MgO layer 10 and the Co of high work content 3o 4layer 30 prepares multilayer conductive film 100, MgO layer 10 is both as cushion and matching layer, the work function of conductive film 100 is obtained improve and there is higher light transmission significantly, conductive film is at 300 ~ 900nm wave-length coverage visible light transmissivity 85% ~ 95%, square resistance scope 2 ~ 15 Ω/, surface work function 5.6 ~ 6.2eV.
The preparation method of above-mentioned conductive film 100, comprises the following steps:
S110, MgO target and substrate are loaded the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, the vacuum of vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -5pa;
Described in present embodiment, MgO target is obtained by following steps: sintered at 800 DEG C ~ 1400 DEG C by MgO powder and make target.
Substrate is glass substrate.Preferably, substrate uses acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning before use.
In present embodiment, the vacuum of vacuum cavity is preferably 6 × 10 -4pa.
Step S120, at described substrate surface sputter MgO layer 10, described in sputter, the technological parameter of MgO layer 10 is: base target spacing is 45mm ~ 85mm, sputtering power is 80W ~ 200W, magnetron sputtering operating pressure 0.2Pa ~ 2Pa, the flow of working gas is 15sccm ~ 35sccm, underlayer temperature is 200 DEG C ~ 700 DEG C, obtains MgO layer 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 450 DEG C.
The thickness of described MgO layer 10 is 40nm ~ 160nm, is preferably 80nm.
Step S130, then MgO film substrate is put into evaporated device cavity, the vacuum regulating vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -6pa,
At the surperficial evaporation conductive layer 20 of described MgO layer 10, described in evaporation, the technological parameter of conductive layer 20 is: evaporation rate 0.5 ~ 3nm/s, evaporation time 10 ~ 80s, and the material of described conductive layer is selected from gold, silver, the one in copper and platinum.
Preferably, evaporation rate 2nm/s, evaporation time 11s.
The thickness of described conductive layer 20 is 5nm ~ 40nm40nm, is preferably 22nm;
Step S140, at the surperficial evaporation Co of described conductive layer 20 3o 4layer 30, Co described in evaporation 3o 4the technological parameter of layer 30 is: evaporation rate 0.2 ~ 2nm/s, evaporation time 5 ~ 50s.
Described Co 3o 4the thickness of layer 30 is 1nm ~ 10nm, is preferably 3.5nm.
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 embodiment, comprise stacked substrate 201, MgO layer 202, conductive layer 203 and Co 3o 4layer 204.
Substrate 201 is glass substrate.The thickness of substrate 201 is 0.1mm ~ 3.0mm, is preferably 1mm.
The thickness of described MgO layer 202 is 40nm ~ 160nm, is preferably 80nm;
The thickness of described conductive layer 203 is 5nm ~ 40nm, is preferably 22nm;
Described Co 3o 4the thickness of layer 204 is 1nm ~ 10nm, is preferably 3.5nm.
The preparation method of the substrate 200 of above-mentioned organic electroluminescence device, comprises the following steps:
S210, MgO target and substrate are loaded the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, the vacuum of vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -5pa; .
In present embodiment, described in present embodiment, MgO target is obtained by following steps: sintered at 800 DEG C ~ 1400 DEG C by MgO powder and make target.
Substrate is glass substrate.Preferably, substrate uses acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning before use.
In present embodiment, the vacuum of vacuum cavity is preferably 6 × 10 -4pa.
Step S220, at described substrate surface sputter MgO layer 202, described in sputter, the technological parameter of MgO layer 202 is: base target spacing is 45mm ~ 85mm, sputtering power is 80W ~ 200W, magnetron sputtering operating pressure 0.2Pa ~ 2Pa, the flow of working gas is 15sccm ~ 35sccm, underlayer temperature is 200 DEG C ~ 700 DEG C, obtains MgO layer 202.
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 450 DEG C.
The thickness of described MgO layer 202 is 40nm ~ 160nm, is preferably 80nm.
Step S203, then MgO layer 202 is put into evaporated device cavity, the vacuum regulating vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -6pa,
At the surperficial evaporation conductive layer 203 of described MgO layer 202, described in evaporation, the technological parameter of conductive layer 203 is: evaporation rate 0.5 ~ 3nm/s, evaporation time 10 ~ 80s, and the material of described conductive layer is selected from gold, silver, the one in copper and platinum.
Preferably, evaporation rate 2nm/s, evaporation time 11s.
The thickness of described conductive layer 203 is 5nm ~ 40nm, is preferably 22nm;
Step S204, at the surperficial evaporation Co of described conductive layer 203 3o 4layer 204, Co described in evaporation 3o 4the technological parameter of layer 204 is: evaporation rate 0.2nm/s ~ 2nm/s, evaporation time 5s ~ 50s.
Described Co 3o 4the thickness of layer 204 is 1nm ~ 10nm, is preferably 3.5nm.
Refer to Fig. 3, the organic electroluminescence device 300 of an embodiment 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 MgO layer 10, conductive layer 20 and Co 3o 4layer 30, wherein, the material of conductive layer is selected from gold, silver, the one in copper and platinum.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.
The thickness of described MgO layer 10 is 40nm ~ 160nm, is preferably 80nm;
The thickness of described conductive layer 20 is 5nm ~ 40nm, is preferably 22nm;
Described Co 3o 4the thickness of layer 30 is 1nm ~ 10nm, is preferably 3.5nm.
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 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 carrier, can luminous efficiency be improved.
Be specific embodiment below.
Embodiment 1
Select purity be 99.9% powder, MgO powder being sintered at 1250 DEG C into diameter is 50mm, and thickness is the MgO ceramic target of 2mm, MgO target is loaded in vacuum cavity.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 50mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 6.0 × 10 -4pa, the working gas flow of argon gas is 20sccm, pressure is adjusted to 1.0Pa, underlayer temperature is 450 DEG C, sputtering power is 100W, and on substrate, sputtering obtains MgO layer, and thickness is 80nm, then MgO layer is put into evaporated device vacuum cavity, with mechanical pump and molecular pump, the vacuum of cavity is extracted into 2.0 × 10 -4pa.Successively evaporation Au film and Co 3o 4film, the evaporation rate of evaporation Au is 2nm/s, evaporation time 11s, evaporation Co 3o 4evaporation rate be 0.5nm/s, evaporation time 7s, deposits the film of 22nm and 3.5nm film respectively, obtains MgO-Au-Co 3o 4the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 9 Ω/, surface work function tester records surface work function 6.0eV.
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 89% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity as seen from Figure 4.
Select MgO-Au-Co 3o 4the transparent conductive film of multilayer as the anode of organic semiconductor device, at evaporation 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 electric current and brightness relationship figure, curve 1 is voltage and current density relation curve in figure 5, device luminescence from 5.0V 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
Select purity be 99.9% powder, MgO powder being sintered at 1400 DEG C into diameter is 50mm, and thickness is the MgO ceramic target of 2mm, MgO target is loaded in vacuum cavity.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 35mm.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 15sccm, pressure is adjusted to 2.0Pa, underlayer temperature is 550 DEG C, sputtering power is 160W, and on substrate, sputtering obtains MgO layer, and thickness is 50nm, then MgO layer is put into evaporated device vacuum cavity, with mechanical pump and molecular pump, the vacuum of cavity is extracted into 1.0 × 10 -6pa.Successively evaporation Au film and Co 3o 4film, the evaporation rate of evaporation Au is 3nm/s, evaporation time 13s, evaporation Co 3o 4evaporation rate be 0.2nm/s, evaporation time 5s, deposits the film of 39nm and 1nm film respectively, obtains MgO-Au-Co 3o 4the 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 5.8eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 89% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 3
Select purity be 99.9% powder, MgO powder being sintered at 800 DEG C into diameter is 50mm, and thickness is the MgO ceramic target of 2mm, MgO target is loaded in vacuum cavity.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 90mm.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 35sccm, pressure is adjusted to 0.2Pa, underlayer temperature is 200 DEG C, sputtering power is 600W, and on substrate, sputtering obtains MgO layer, and thickness is 150nm, then MgO layer is put into evaporated device vacuum cavity, with mechanical pump and molecular pump, the vacuum of cavity is extracted into 1.0 × 10 -3pa.Successively evaporation Au film and Co 3o 4film, the evaporation rate of evaporation Au is 0.5nm/s, evaporation time 10s, evaporation Co 3o 4evaporation rate be 0.5nm/s, evaporation time 10s, deposits the film of 5nm and 5nm film respectively, obtains MgO-Au-Co 3o 4the 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 6.1eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 93% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 4
Select purity be 99.9% powder, MgO powder being sintered at 1250 DEG C into diameter is 50mm, and thickness is the MgO ceramic target of 2mm, MgO target is loaded in vacuum cavity.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 50mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 6.0 × 10 -4pa, the working gas flow of argon gas is 20sccm, pressure is adjusted to 1.0Pa, underlayer temperature is 700 DEG C, sputtering power is 100W, and on substrate, sputtering obtains MgO layer, and thickness is 80nm, then MgO layer is put into evaporated device vacuum cavity, with mechanical pump and molecular pump, the vacuum of cavity is extracted into 2.0 × 10 -4pa.Successively evaporation Ag film and Co 3o 4film, the evaporation rate of evaporation Ag is 2.5nm/s, evaporation time 16s, evaporation Co 3o 4evaporation rate be 0.2nm/s, evaporation time 15s, deposits the film of 40nm and 3nm film respectively, obtains MgO-Ag-Co 3o 4the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 9 Ω/, surface work function tester records surface work function 6.0eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 89% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 5
Select purity be 99.9% powder, MgO powder being sintered at 950 DEG C into diameter is 50mm, and thickness is the MgO ceramic target of 2mm, MgO target is loaded in vacuum cavity.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 35mm.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 15sccm, pressure is adjusted to 2.0Pa, underlayer temperature is 300 DEG C, sputtering power is 160W, and on substrate, sputtering obtains MgO layer, and thickness is 70nm, then MgO layer is put into evaporated device vacuum cavity, with mechanical pump and molecular pump, the vacuum of cavity is extracted into 1.0 × 10 -6pa.Successively evaporation Ag film and Co 3o 4film, the evaporation rate of evaporation Ag is 0.4nm/s, evaporation time 80s, evaporation Co 3o 4evaporation rate be 0.4nm/s, evaporation time 20s, deposits the film of 32nm and 8nm film respectively, obtains MgO-Ag-Co 3o 4the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 9 Ω/, surface work function tester records surface work function 5.7eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 81% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 6
Select purity be 99.9% powder, MgO powder being sintered at 900 DEG C into diameter is 50mm, and thickness is the MgO ceramic target of 2mm, MgO target is loaded in vacuum cavity.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 90mm.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 35sccm, pressure is adjusted to 0.2Pa, underlayer temperature is 400 DEG C, sputtering power is 600W, and on substrate, sputtering obtains MgO layer, and thickness is 100nm, then MgO layer is put into evaporated device vacuum cavity, with mechanical pump and molecular pump, the vacuum of cavity is extracted into 1.0 × 10 -3pa.Successively evaporation Ag film and Co 3o 4film, the evaporation rate of evaporation Ag is 1nm/s, evaporation time 20, evaporation Co 3o 4evaporation rate be 0.5nm/s, evaporation time 8s, deposits the film of 20nm and 4nm film respectively, obtains MgO-Ag-Co 3o 4the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 15 Ω/, surface work function tester records surface work function 6.2eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 92% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 7
Select purity be 99.9% powder, MgO powder being sintered at 1000 DEG C into diameter is 50mm, and thickness is the MgO ceramic target of 2mm, MgO target is loaded in vacuum cavity.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 50mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 6.0 × 10 -4pa, the working gas flow of argon gas is 20sccm, pressure is adjusted to 1.0Pa, underlayer temperature is 600 DEG C, sputtering power is 100W, and on substrate, sputtering obtains MgO layer, and thickness is 120nm, then MgO layer is put into evaporated device vacuum cavity, with mechanical pump and molecular pump, the vacuum of cavity is extracted into 2.0 × 10 -4pa.Successively evaporating Cu film and Co 3o 4film, the evaporation rate of evaporation Cu is 0.4nm/s, evaporation time 50s, evaporation Co 3o 4evaporation rate be 0.5nm/s, evaporation time 7s, deposits the film of 22nm and 3.5nm film respectively, obtains MgO-Cu-Co 3o 4the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 9 Ω/, surface work function tester records surface work function 6.0eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 89% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 8
Select purity be 99.9% powder, MgO powder being sintered at 1350 DEG C into diameter is 50mm, and thickness is the MgO ceramic target of 2mm, MgO target is loaded in vacuum cavity.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 35mm.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 15sccm, pressure is adjusted to 2.0Pa, underlayer temperature is 650 DEG C, sputtering power is 160W, and on substrate, sputtering obtains MgO layer, and thickness is 80nm, then MgO layer is put into evaporated device vacuum cavity, with mechanical pump and molecular pump, the vacuum of cavity is extracted into 1.0 × 10 -6pa.Successively evaporating Cu film and Co 3o 4film, the evaporation rate of evaporation Cu is 1.5nm/s, evaporation time 20s, evaporation Co 3o 4evaporation rate be 0.2nm/s, evaporation time 6s, deposits the film of 30nm and 1.2nm film respectively, obtains MgO-Cu-Co 3o 4the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 9 Ω/, surface work function tester records surface work function 5.7eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 81% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 9
Select purity be 99.9% powder, MgO powder being sintered at 900 DEG C into diameter is 50mm, and thickness is the MgO ceramic target of 2mm, MgO target is loaded in vacuum cavity.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 90mm.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 35sccm, pressure is adjusted to 0.2Pa, underlayer temperature is 500 DEG C, sputtering power is 600W, and on substrate, sputtering obtains MgO layer, and thickness is 110nm, then MgO layer is put into evaporated device vacuum cavity, with mechanical pump and molecular pump, the vacuum of cavity is extracted into 1.0 × 10 -3pa.Successively evaporating Cu film and Co 3o 4film, the evaporation rate of evaporation Cu is 1.5nm/s, evaporation time 10s, evaporation Co 3o 4evaporation rate be 0.5nm/s, evaporation time 5s, deposits the film of 15nm and 2.5nm film respectively, obtains MgO-Cu-Co 3o 4the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 15 Ω/, surface work function tester records surface work function 6.2eV.
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 10
Select purity be 99.9% powder, MgO powder being sintered at 1250 DEG C into diameter is 50mm, and thickness is the MgO ceramic target of 2mm, MgO target is loaded in vacuum cavity.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 50mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 6.0 × 10 -4pa, the working gas flow of argon gas is 20sccm, pressure is adjusted to 1.0Pa, underlayer temperature is 450 DEG C, sputtering power is 100W, and on substrate, sputtering obtains MgO layer, and thickness is 120nm, then MgO layer is put into evaporated device vacuum cavity, with mechanical pump and molecular pump, the vacuum of cavity is extracted into 2.0 × 10 -4pa.Successively evaporation Pt film and Co 3o 4film, the evaporation rate of evaporation Pt is 0.4nm/s, evaporation time 55s, evaporation Co 3o 4evaporation rate be 2nm/s, evaporation time 5s, deposits the film of 22nm and 10nm film respectively, obtains MgO-Pt-Co 3o 4the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 9 Ω/, surface work function tester records surface work function 6.0eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 89% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 11
Select purity be 99.9% powder, MgO powder being sintered at 1350 DEG C into diameter is 50mm, and thickness is the MgO ceramic target of 2mm, MgO target is loaded in vacuum cavity.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 35mm.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 15sccm, pressure is adjusted to 2.0Pa, underlayer temperature is 250 DEG C, sputtering power is 160W, and on substrate, sputtering obtains MgO layer, and thickness is 80nm, then MgO layer is put into evaporated device vacuum cavity, with mechanical pump and molecular pump, the vacuum of cavity is extracted into 1.0 × 10 -6pa.Successively evaporation Pt film and Co 3o 4film, the evaporation rate of evaporation Pt is 1.5nm/s, evaporation time 20s, evaporation Co 3o 4evaporation rate be 0.3nm/s, evaporation time 10s, deposits the film of 30nm and 3nm film respectively, obtains MgO-Pt-Co 3o 4the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 9 Ω/, surface work function tester records surface work function 5.7eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 81% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
Embodiment 12
Select purity be 99.9% powder, MgO powder being sintered at 900 DEG C into diameter is 50mm, and thickness is the MgO ceramic target of 2mm, MgO target is loaded in vacuum cavity.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 90mm.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 35sccm, pressure is adjusted to 0.2Pa, underlayer temperature is 400 DEG C, sputtering power is 600W, and on substrate, sputtering obtains MgO layer, and thickness is 90nm, then MgO layer is put into evaporated device vacuum cavity, with mechanical pump and molecular pump, the vacuum of cavity is extracted into 1.0 × 10 -3pa.Successively evaporation Pt film and Co 3o 4film, the evaporation rate of evaporation Pt is 0.5nm/s, evaporation time 20s, evaporation Co 3o 4evaporation rate be 0.2nm/s, evaporation time 15s, deposits the film of 10nm and 3nm film respectively, obtains MgO-Pt-Co 3o 4the transparent conductive film of multilayer.
Test result: adopt four point probe resistance meter to record square resistance 33 Ω/, surface work function tester records surface work function 6.0eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300 ~ 900nm.Film reaches 89% at visible ray 470 ~ 790nm wave-length coverage mean transmissivity.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.

Claims (10)

1. a conductive film, is characterized in that, comprises stacked MgO layer, conductive layer and Co 3o 4layer, wherein the material of conductive layer is selected from gold, silver, the one in copper and platinum.
2. conductive film according to claim 1, is characterized in that, the thickness of described MgO layer is 40nm ~ 160nm, and the thickness of described conductive layer is 5nm ~ 40nm, described Co 3o 4the thickness of layer is 1nm ~ 10nm.
3. a preparation method for conductive film, is characterized in that, comprises the following steps:
MgO target and substrate are loaded the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, the vacuum of vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -5pa;
At described substrate surface sputter MgO layer, described in sputter, the technological parameter of MgO layer is: base target spacing is 45mm ~ 85mm, sputtering power is 80W ~ 200W, magnetron sputtering operating pressure 0.2Pa ~ 2Pa, the flow of working gas is 15sccm ~ 35sccm, underlayer temperature is 200 DEG C ~ 700 DEG C, obtains MgO film substrate;
Then MgO film substrate is put into evaporated device cavity, the vacuum regulating vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -6pa,
At described MgO layer surface evaporation conductive layer, the technological parameter of conductive layer described in evaporation is: evaporation rate 0.5 ~ 3nm/s, evaporation time 10 ~ 80s, and the material of described conductive layer is selected from gold, silver, the one in copper and platinum;
At described conductive layer surface evaporation Co 3o 4layer, Co described in evaporation 3o 4the technological parameter of layer is: evaporation rate 0.2 ~ 2nm/s, evaporation time 5 ~ 50s, and
Peel off described substrate, obtain described lamination conductive film.
4. the preparation method of conductive film according to claim 3, is characterized in that, described MgO target is obtained by following steps: sintered at 800 DEG C ~ 1400 DEG C by MgO powder and make target.
5. the preparation method of conductive film according to claim 3, is characterized in that, the thickness of described MgO layer is 40nm ~ 160nm, and the thickness of described conductive layer is 5nm ~ 40nm, described Co 3o 4the thickness of layer is 1nm ~ 10nm.
6. a substrate for organic electroluminescence device, is characterized in that, comprises the substrate stacked gradually, stacked MgO layer, conductive layer and Co 3o 4layer, wherein the material of conductive layer is selected from gold, silver, the one in copper and platinum.
7. the substrate of organic electroluminescence device according to claim 6, is characterized in that, the thickness of described MgO layer is 40nm ~ 160nm, and the thickness of described conductive layer is 5nm ~ 40nm, described Co 3o 4the 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:
MgO target and substrate are loaded the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, the vacuum of vacuum cavity is 1.0 × 10 -3pa ~ 1.0 × 10 -5pa;
At described substrate surface sputter MgO layer, described in sputter, the technological parameter of MgO layer is: base target spacing is 45mm ~ 85mm, sputtering power is 80W ~ 200W, magnetron sputtering operating pressure 0.2Pa ~ 2Pa, the flow of working gas is 15sccm ~ 35sccm, underlayer temperature is 200 DEG C ~ 700 DEG C, obtains MgO film substrate;
Then MgO film substrate is put into evaporated device cavity, the vacuum regulating vacuum cavity is 1.0 × 10 -3p a~ 1.0 × 10 -6pa,
At described MgO layer surface evaporation conductive layer, the technological parameter of conductive layer described in evaporation is: evaporation rate 0.5 ~ 3nm/s, evaporation time 10 ~ 80s, and the material of described conductive layer is selected from gold, silver, the one in copper and platinum;
At described conductive layer surface evaporation Co 3o 4layer, Co described in evaporation 3o 4the technological parameter of layer is: evaporation rate 0.2 ~ 2nm/s, evaporation time 5 ~ 50s.
9. the preparation method of the substrate of organic electroluminescence device according to claim 8, is characterized in that, described MgO target is obtained by following steps: sintered at 800 DEG C ~ 1400 DEG C by MgO powder and make 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 stacked MgO layer, conductive layer and Co 3o 4layer, wherein the material of conductive layer is selected from gold, silver, the one in copper and platinum.
CN201310337079.2A 2013-08-05 2013-08-05 Conductive film, and preparation method and application thereof Pending CN104339746A (en)

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