CN106098960A - A kind of conductive film, its preparation method and application thereof - Google Patents
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Abstract
A kind of conductive film, including Ag layer and the L of stacking2O3Layer, wherein, L is europium element, samarium element, yttrium, gadolinium element, the one in neodymium element.Above-mentioned conductive film is by depositing and the L of high work content on the surface of Ag layer2O3Layer prepares bilayer conductive thin film, can keep the good electric conductivity of Ag layer, make again the work function of conductive film obtain significant raising.The present invention also provides for the preparation method and application of a kind of conductive film.
Description
Technical field
The present invention relates to photoelectric semiconductor material, particularly relate to conductive film, its preparation method, use this conductive film
The substrate of organic electroluminescence device, 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 Aska-Rid. is Recent study widest transparent conductive film material
Material, has higher visible light transmittance rate and low resistivity.But the luminous efficiency of device to be improved, it is desirable to transparent conductive film
Anode has higher surface work function.And the work function of the zinc oxide of aluminum, gallium and indium doping typically only has 4.3eV, through UV
Light radiation or ozone etc. also can only achieve 4.0～4.3eV after processing, with the lumo energy (typical case of general organic luminous layer
For 2.8～4.2eV) also have the biggest energy level difference away from, cause the increase of carrier injection barrier, carrying of obstruction luminous efficiency
High.
Summary of the invention
Based on this, it is necessary to for the problem that conductive film work function is relatively low, it is provided that the electrically conducting transparent of a kind of nano wire is thin
Film, its preparation method, use the substrate of the organic electroluminescence device of this conductive film, its preparation method and organic electroluminescent
Device.
A kind of conductive film, including Ag layer and the L of stacking2O3Layer.
Described conductive film is the conductive film of nano thread structure, and described L is europium element, samarium element, yttrium, gadolinium unit
Element, the one in neodymium element.
The thickness of described Ag layer is 5nm～20nm, described L2O3The thickness of layer is 0.5nm～5nm.
The preparation method of a kind of conductive film, comprises the following steps:
By Ag target and L2O3Target and substrate load the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, vacuum cavity
Vacuum is 1.0 × 10-3Pa～1.0 × 10-5Pa；
At described substrate surface sputter Ag layer, described in sputter, the technological parameter of Ag layer is: base target spacing is 45mm～95mm,
The energy of laser is 80W～300W, and pressure is 3Pa～30Pa, is passed through noble gas, the flow of noble gas be 10sccm～
40sccm, underlayer temperature is 250 DEG C～750 DEG C；
At described Ag layer surface sputter L2O3Layer, L described in sputter2O3Layer technological parameter be: base target spacing be 45mm～
95mm, the energy of laser is 80W～300W, and pressure is 3Pa～30Pa, is passed through noble gas, and the flow of noble gas is
10sccm～40sccm, underlayer temperature is 250 DEG C～750 DEG C；And
Peel off described substrate, obtain described conductive film.
The substrate of a kind of organic electroluminescence device, including the substrate stacked gradually, the Ag layer of stacking and L2O3 layer.
Conductive film in described substrate is the conductive film of nano thread structure, and described nanowire diameter is 5nm～25nm.
The preparation method of the substrate of a kind of organic electroluminescence device, comprises the following steps:
By Ag target and L2O3Target and substrate load the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, vacuum cavity
Vacuum is 1.0 × 10-3Pa～1.0 × 10-5Pa；
At described substrate surface sputter Ag layer, described in sputter, the technological parameter of Ag layer is: base target spacing is 45mm～95mm,
The energy of laser is 80W～300W, and pressure is 3Pa～30Pa, is passed through noble gas, the flow of noble gas be 10sccm～
40sccm, underlayer temperature is 250 DEG C～750 DEG C；
At described Ag layer surface sputter L2O3Layer, L described in sputter2O3Layer technological parameter be: base target spacing be 45mm～
95mm, the energy of laser is 80W～300W, and pressure is 3Pa～30Pa, is passed through noble gas, and the flow of noble gas is
10sccm～40sccm, underlayer temperature is 250 DEG C～750 DEG C.
A kind of organic electroluminescence device, including the anode stacked gradually, luminescent layer and negative electrode, described anode includes layer
Folded Ag layer and L2O3Layer.
Above-mentioned conductive film by depositing L on the surface of Ag layer2O3Layer prepares bilayer conductive thin film, can keep Ag layer
Good electric conductivity, makes again the work function of conductive film obtain significant raising, and conductive film is at 300～900nm wavelength
Scope visible light transmissivity 80%～95%, square resistance scope 10～35 Ω/, surface work function 5.3～5.8eV；Above-mentioned
The preparation method of conductive film, uses laser ablation target, makes the ablated one-tenth atom of the material in target or the particle of ion cluster,
During particle deposits in substrate, by being passed through substantial amounts of noble gas, make particle be passivated, substrate disperse nucleation,
Then at each nucleating point vertical-growth, the pillared nano wire of shape；Use this conductive film as organic electroluminescence device
Anode, between surface work function and the lumo energy of general organic luminous layer of conductive film, gap is less, reduces load
The injection barrier of stream, can significantly improve 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 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 the conductive film of embodiment 1 preparation；
Detailed description of the invention
Below in conjunction with the accompanying drawings with specific embodiment to conductive film, its preparation method, use the Organic Electricity of this conductive film
The substrate of electroluminescence device, its preparation method and organic electroluminescence device are further elucidated with.
Referring to Fig. 1, the conductive film 100 of an embodiment includes the Ag layer 10 and L of stacking2O3Layer 30.
Described conductive film 100 is the conductive film of nano thread structure, and described nanowire diameter is 5nm～25nm, preferably
For 14nm.
The thickness of described Ag layer 10 is 5nm～20nm, preferably 12nm,
Described L2O3The thickness of layer 30 is 0.5nm～5nm, preferably 2nm.
Above-mentioned conductive film 100 by depositing L on the surface of Ag layer 102O3Layer 30 prepares bilayer conductive thin film, can keep
The good electric conductivity of Ag layer 10, makes again the work function of conductive film 100 obtain significant raising, and conductive film 100 exists
300～900nm wave-length coverage visible light transmissivities 80%～95%, square resistance scope 10～35 Ω/, surface work function
2.8～4.2eV.
The preparation method of above-mentioned conductive film 100, comprises the following steps:
S110, by Ag target and L2O3Target and substrate load the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, vacuum
The vacuum of cavity is 1.0 × 10-3Pa～1.0 × 10-5Pa。
Substrate is glass substrate.Preferably, substrate is before use with acetone, dehydrated alcohol and deionized water ultrasonic cleaning.
In present embodiment, the vacuum of vacuum cavity is preferably 5 × 10-4Pa。
Step S120, at substrate surface sputter Ag layer 10, the technological parameter of sputter Ag layer 10 is: base target spacing be 45mm～
95mm, the energy of laser is 80W～300W, and pressure is 3Pa～30Pa, is passed through noble gas, and the flow of noble gas is
10sccm～40sccm, underlayer temperature is 250 DEG C～750 DEG C.
Preferably, base target spacing is 60mm, and the energy of laser is 150W, and pressure is 10Pa, and noble gas is argon, inertia
The flow of gas is 20sccm, and underlayer temperature is 500 DEG C.
The thickness of the Ag layer 10 formed is 5nm～20nm, preferably 12nm.
Step S130, at Ag layer 10 surface sputter L2O3Layer 30, magnetron sputtering L2O3The technological parameter of layer 30 is: between base target
Away from for 45mm～95mm, the energy of laser is 80W～300W, and pressure is 3Pa～30Pa, is passed through noble gas, noble gas
Flow is 10sccm～40sccm, and underlayer temperature is 250 DEG C～750 DEG C；
Form L2O3The thickness of layer 30 is 0.5nm～5nm, preferably 2nm.
At the bottom of step S140, peeling liner, obtain conductive film 100.
The preparation method of above-mentioned conductive film, use laser ablation target, make the ablated one-tenth atom of the material in target or
The particle of ion cluster, during particle deposits in substrate, by being passed through substantial amounts of noble gas, makes particle be passivated, at base
Nucleation, then at each nucleating point vertical-growth, the pillared nano wire of shape is disperseed on plate.Can be by regulation noble gas pressure
Strong size controls thickness and the distance between centers of tracks of nano wire.Being passed through noble gas pressure big, the nano wire obtained is relatively thin, between line
Away from bigger.
Referring to Fig. 2, the substrate 200 of the organic electroluminescence device of an embodiment, including substrate 201, the Ag of stacking
Layer 202 and L2O3Layer 203.
Substrate 201 is glass substrate.The thickness of substrate 201 is 0.1mm～3.0mm, preferably 1mm.
Ag layer 202 and L2O3Layer 203 is the conductive film of nano thread structure, and described nanowire diameter is 5nm～25nm
The thickness of Ag layer 202 is 5nm～20nm, preferably 12nm.
L2O3The thickness of layer 203 is 0.5nm～5nm, preferably 2nm.
The substrate 200 of above-mentioned organic electroluminescence device by depositing L on the surface of Ag layer 2022O3Layer 203 preparation multilamellar
Conductive film, can keep the good electric conductivity of Ag layer 202, makes again the work content of the substrate 200 of organic electroluminescence device
Number has obtained significant raising, and the substrate 200 of organic electroluminescence device is at 300～900nm wave-length coverage visible light transmissivities
80%～95%, square resistance scope 10～35 Ω/, surface work function 2.8～4.2eV.
The preparation method of the substrate 200 of above-mentioned organic electroluminescence device, comprises the following steps:
S210, by Ag target and L2O3Target and substrate 201 load the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, very
The vacuum of cavity body is 1.0 × 10-3Pa～1.0 × 10-5Pa。
Substrate is glass substrate.Preferably, substrate is before use with acetone, dehydrated alcohol and deionized water ultrasonic cleaning.
In present embodiment, the vacuum of vacuum cavity is preferably 5 × 10-4Pa。
Step S220, at substrate surface sputter Ag layer 202, the technological parameter of sputter AZO layer 202 is: base target spacing is
45mm～95mm, the energy of laser is 80W～300W, and pressure is 3Pa～30Pa, is passed through noble gas, the flow of noble gas
For 10sccm～40sccm, underlayer temperature is 250 DEG C～750 DEG C.
Preferably, base target spacing is 60mm, and the energy of laser is 150W, and pressure is 10Pa, and noble gas is argon, inertia
The flow of gas is 20sccm, and underlayer temperature is 500 DEG C.
The thickness of the Ag layer 10 formed is 5nm～20nm, preferably 12nm.
Step S203, at Ag layer 202 surface sputter L2O3The technological parameter of layer 203 is: base target spacing is 45mm～95mm,
The energy of laser is 80W～300W, and pressure is 3Pa～30Pa, is passed through noble gas, the flow of noble gas be 10sccm～
40sccm, underlayer temperature is 250 DEG C～750 DEG C
The preparation method of the substrate 200 of above-mentioned organic electroluminescence device, uses laser ablation target, makes the material in target
Expect ablated one-tenth atom or the particle of ion cluster, during particle deposits in substrate, by being passed through substantial amounts of noble gas,
Make particle be passivated, substrate disperses nucleation, then at each nucleating point vertical-growth, the pillared nano wire of shape.Can lead to
Overregulate the size of noble gas pressure to control thickness and the distance between centers of tracks of nano wire.It is passed through noble gas pressure big, obtains
Nano wire relatively thin, distance between centers of tracks is relatively big, prepares Ag layer 202 and L on the substrate 2012O3Layer, technique is relatively simple.
Referring to Fig. 3, the organic electroluminescence device 300 of an embodiment includes substrate 301, the anode stacked gradually
302, luminescent layer 303 and negative electrode 304.Anode 302 is made up of conductive film 100, including the L of the Ag layer 10 of stacking2O3Layer 30.
Substrate 301 is glass substrate, it will be understood that according to the difference of organic electroluminescence device 300 concrete structure, substrate 301 is permissible
Omit.The material of luminescent layer 303 is 4-(dintrile methyl)-2-butyl-6-(1,1,7,7-tetramethyl long Lip river pyridine-9-ethylene
Base)-4H-pyrans (DCJTB), 9,10-bis--β-naphthylene anthracene (AND), two (2-methyl-8-hydroxyquinoline)-(4-xenol) aluminum
(BALQ), 4-(dintrile methene)-2-isopropyl-6-(1,1,7,7-tetramethyl long Lip river pyridine-9-vinyl)-4H-pyrans
(DCJTI), dimethylquinacridone (DMQA), 8-hydroxyquinoline aluminum (Alq3), double (4,6-difluorophenyl pyridinato-N, C2) pyrrole
Pyridine formyl closes iridium (FIrpic), two (2-methyl-diphenyl [f, h] quinoxaline) (acetylacetone,2,4-pentanedione) closes iridium (Ir (MDQ)2(acac))
Or three (2-phenylpyridine) closes iridium (Ir (ppy)3).The material of negative electrode 304 is silver (Ag), gold (Ag), aluminum (Al), platinum (Pt) or magnesium
Silver alloy.
The thickness of described Ag layer 10 is 5nm～20nm, preferably 12nm,
Described L2O3The thickness of layer 30 is 0.5nm～5nm, preferably 2nm.
It is appreciated that above-mentioned organic electroluminescence device 300 arranges other functional layers also dependent on use demand.
Above-mentioned organic electroluminescence device 300, uses conductive film 100 as the anode of organic electroluminescence device, leads
The surface work function 4.0～4.3eV of conductive film, with the lumo energy (typically 2.8～4.2eV) of general organic luminous layer
Between gap less, reduce the injection barrier of carrier, luminous efficiency can be improved.
It is specific embodiment below.
Embodiment 1
Argent powder and the Eu selecting purity to be 99.9%2O3Powder is respectively implanted in two porcelain boats, then is loaded by porcelain boat
In vacuum cavity.Then, successively by acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass substrate, vacuum cavity is put into.?
The distance of target and substrate is set as 60mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 5.0 × 10-4Pa, argon
Working gas flow be 20sccm, pressure is adjusted to 10Pa, and underlayer temperature is 500 DEG C, and laser energy is 150W.Successively sputtering
Ag target and Eu2O3Target, deposits the thin film of 12nm and 2nm thin film respectively, obtains Ag-Eu2O3Double-deck transparent conductive film.
Test result: using four probe instrument to record square resistance 10 Ω/, surface work function tester records
Surface work function 2.8eV.
Refer to Fig. 4, Fig. 4 and show the transmitted spectrum of the transparent conductive film obtained, use UV, visible light spectrophotometric
Measurement examination, test wavelength is 300～900nm.Thin film is the most saturating in visible ray 470～790nm wave-length coverage as seen from Figure 4
Rate of crossing has reached 90%.
Select Ag-Eu2O3The transparent conductive film of multilamellar, as the anode of organic semiconductor device, is deposited with luminescence above
Layer Alq3, and negative electrode employing Ag, prepare organic electroluminescence device.
Embodiment 2
Argent powder and the Eu selecting purity to be 99.9%2O3Powder is respectively implanted in two porcelain boats, then is loaded by porcelain boat
In vacuum cavity.Then, successively by acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass substrate, vacuum cavity is put into.?
The distance of target and substrate is set as 45mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 1.0 × 10-5Pa, argon
Working gas flow be 10sccm, pressure is adjusted to 3Pa, and underlayer temperature is 250 DEG C, and laser energy is 300W.Successively sputtering
Ag target and Eu2O3Target, deposits the thin film of 20nm and 0.5nm thin film respectively, obtains Ag-Eu2O3The electrically conducting transparent of multilamellar is thin
Film.
Test result: using four probe instrument to record square resistance 15 Ω/, surface work function tester records
Surface work function 2.9eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300～900nm.Thin film at visible ray 470～
790nm wave-length coverage mean transmissivity has reached 88%.
Embodiment 3
Aurum metallicum powder body and the CaO powder of selecting purity to be 99.9% are respectively implanted in two porcelain boats, then are loaded by porcelain boat
In vacuum cavity.Then, successively by acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass substrate, vacuum cavity is put into.?
The distance of target and substrate is set as 95mm.With mechanical pump and molecular pump, the vacuum of cavity is extracted into 1.0 × 10-3Pa, argon
Working gas flow be 40sccm, pressure is adjusted to 30Pa, and underlayer temperature is 750 DEG C, and laser energy is 80W.Successively sputtering
Ag target and Eu2O3Target, deposits the thin film of 10nm and 5nm thin film respectively, obtains Ag-Eu2O3The transparent conductive film of multilamellar.
Test result: using four probe instrument to record square resistance 330 Ω/, surface work function tester is surveyed
Obtain surface work function 3.1eV.
Use ultraviolet-uisible spectrophotometer is tested, and test wavelength is 300～900nm.Thin film at visible ray 470～
790nm wave-length coverage mean transmissivity has reached 90%.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but also
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that, for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (8)
1. a conductive film, it is characterised in that include Ag layer and the L of stacking2O3Layer.
Conductive film the most according to claim 1, it is characterised in that described L is europium element, samarium element, yttrium, gadolinium unit
Element, the one in neodymium element.
Conductive film the most according to claim 1, it is characterised in that the thickness of described Ag layer is 5nm～20nm, described
L2O3The thickness of layer is 0.5nm～5nm.
4. the preparation method of a conductive film, it is characterised in that comprise the following steps:
By Ag target and L2O3Target and substrate load the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, the vacuum of vacuum cavity
Degree is 1.0 × 10-3Pa～1.0 × 10-5Pa；
At described substrate surface sputter Ag layer, described in sputter, the technological parameter of Ag layer is: base target spacing is 45mm～95mm, laser
Energy be 80W～300W, pressure is 3Pa～30Pa, is passed through noble gas, the flow of noble gas be 10sccm～
40sccm, underlayer temperature is 250 DEG C～750 DEG C；
At described Ag layer surface sputter L2O3Layer, L described in sputter2O3The technological parameter of layer is: base target spacing is 45mm～95mm, swashs
The energy of light is 80W～300W, and pressure is 3Pa～30Pa, is passed through noble gas, the flow of noble gas be 10sccm～
40sccm, underlayer temperature is 250 DEG C～750 DEG C；And
Peel off described substrate, obtain described conductive film.
5. the substrate of an organic electroluminescence device, it is characterised in that include substrate, Ag layer and the L stacked gradually2O3Layer.
The substrate of organic electroluminescence device the most according to claim 5, it is characterised in that the conductive thin in described substrate
Film is the conductive film of nano thread structure, and described nanowire diameter is 5nm～25nm.
7. the preparation method of the substrate of an organic electroluminescence device, it is characterised in that comprise the following steps:
By Ag target and L2O3Target and substrate load the vacuum cavity of magnetic-controlled sputtering coating equipment, wherein, the vacuum of vacuum cavity
Degree is 1.0 × 10-3Pa～1.0 × 10-5Pa；
At described substrate surface sputter Ag layer, described in sputter, the technological parameter of Ag layer is: base target spacing is 45mm～95mm, laser
Energy be 80W～300W, pressure is 3Pa～30Pa, is passed through noble gas, the flow of noble gas be 10sccm～
40sccm, underlayer temperature is 250 DEG C～750 DEG C；
At described Ag layer surface sputter L2O3Layer, L described in sputter2O3The technological parameter of layer is: base target spacing is 45mm～95mm, swashs
The energy of light is 80W～300W, and pressure is 3Pa～30Pa, is passed through noble gas, the flow of noble gas be 10sccm～
40sccm, underlayer temperature is 250 DEG C～750 DEG C.
8. an organic electroluminescence device, including the anode stacked gradually, luminescent layer and negative electrode, it is characterised in that described
Anode includes Ag layer and the L of stacking2O3Layer.
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