CN104700922A - Multilayer transparent conductive thin film, production method thereof and electroluminescent device - Google Patents
Multilayer transparent conductive thin film, production method thereof and electroluminescent device Download PDFInfo
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- CN104700922A CN104700922A CN201310671841.0A CN201310671841A CN104700922A CN 104700922 A CN104700922 A CN 104700922A CN 201310671841 A CN201310671841 A CN 201310671841A CN 104700922 A CN104700922 A CN 104700922A
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Abstract
The invention relates to a multilayer transparent conductive thin film, a production method thereof and an electroluminescent device. The multilayer transparent conductive thin film comprises a buffer matching layer, a conductive layer and a low-work-content layer, wherein the buffer matching layer is made of MeO, and Me is Mg, Zn or Cd; the conductive layer is made of Au; the low-work-content layer is made of R2O, and R is Li, Na, K, Rb or Cs; the buffer matching layer is 50-150 nanometers in thickness; the conductive layer is 5-35 nanometers in thickness; the low-work-content layer is 1-10 nanometers in thickness. The multilayer transparent conductive thin film has the advantages that the multilayer thin film is used as a transparent conductive thin film system, the light transmittance, conductivity and surface work function of the thin film can be respectively adjusted by the layers of the thin film; the production method of the thin film is simple, good reproducibility is achieved, the thin film is suitable for being used as the cathode layer of devices such as an organic electroluminescent device OLED and an solar cell, and the light emitting efficiency can be increased evidently.
Description
Technical field
The present invention relates to photoelectric semiconductor material technical field, particularly relate to multi-layer transparent electroconductive film and preparation method thereof.The invention still further relates to the electroluminescent device applying described multi-layer transparent electroconductive film.
Background technology
Transparent conductive film is photoelectric material optical clear performance and electric conductivity being compounded in one, because it has excellent photoelectric characteristic, becomes study hotspot in recent years and advanced subject, solar cell can be widely used in, the field of screen display such as LED, TFT, LCD and touch-screen.Along with the raising of device performance requirements, the performance for the nesa coating as device cathodes is also requiring to improve.Except keeping high visible transmitance, low resistivity, also requiring lower surface work function, the energy level of itself and other functional layer being matched, reduces potential barrier, improving Carrier Injection Efficiency, finally reach high electrical efficiency.
Transparent 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 zinc 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 negative electrode has lower surface work function.And the zinc oxide of aluminium, gallium and indium doping, work function is generally 4.3eV, 4.0 ~ 4.3eV can be reached after process, larger energy level difference distance is also had with the lumo energy (being typically 2.8 ~ 4.2eV) of general organic luminous layer, cause the increase of carrier injection potential barrier, hinder the raising of luminous efficiency.
Alkali-metal oxide R
2o(R=Li, Na, K, Rb, Cs), have lower surface work function (2.3 ~ 3.0eV), Many researchers is all wished the negative electrode of this kind of material for OLED and solar cell.But the film that these materials are made is all nonconducting, directly nesa coating can not be used as.
Summary of the invention
The object of the invention is to provide a kind of multi-layer transparent electroconductive film, in order to solve existing Thin film conductive performance and work function not high, during as negative electrode, the problem that luminous efficiency is on the low side.
For above-mentioned purpose, the present invention proposes a kind of multi-layer transparent electroconductive film, and it forms by cushioning matching layer, conductive layer and low work function layer, and wherein, the material of described buffering matching layer is MeO, Me is Mg, Zn or Cd; The material of described conductive layer is Au; The material of described low work function layer is R
2o, R are Li, Na, K, Rb or Cs.
Described multi-layer transparent electroconductive film, wherein, the thickness of described buffering matching layer is 50 ~ 150nm; The thickness of described conductive layer is 5 ~ 35nm; The thickness of described low work function layer is 1 ~ 10nm.
Described multi-layer transparent electroconductive film, wherein, the thickness of described buffering matching layer is 80nm; The thickness of described conductive layer is 25nm; The thickness of described low work function layer is 2nm.
Another goal of the invention of the present invention is the preparation method providing multi-layer transparent electroconductive film.
For above-mentioned purpose, the present invention proposes a kind of preparation method of multi-layer transparent electroconductive film, and it comprises the steps:
A () chooses MeO, Au and R respectively
2the powder of O, as target, loads in the vacuum cavity of filming equipment together with substrate;
B the vacuum degree of described vacuum cavity is evacuated to 1.0 × 10 by ()
-3pa ~ 1.0 × 10
-5pa, the spacing adjusting described substrate and described target is 35 ~ 95mm;
(c) over the substrate successively evaporation prepare MeO, Au and R
2o, described evaporation rate is 0.3 ~ 5nm/s;
Wherein, Me is Mg, Zn or Cd; R is Li, Na, K, Rb or Cs;
In described step (c), the evaporation rate of described MeO is 1 ~ 8nm/s, and the evaporation rate of described Au is 0.5 ~ 5nm/s, described R
2the evaporation rate of O is 0.3 ~ 3nm/s.
In described preparation method, the thickness of described buffering matching layer is 50 ~ 150nm; The thickness of described conductive layer is 5 ~ 35nm; The thickness of described low work function layer is 1 ~ 10nm.
Further, in described preparation method, the thickness of described buffering matching layer is 80nm; The thickness of described conductive layer is 25nm; The thickness of described low work function layer is 2nm.
Another goal of the invention of the present invention is to provide a kind of electroluminescent device.
For above-mentioned purpose, the present invention also proposes a kind of electroluminescent device, described straticulate structure is followed successively by glass substrate, cathode layer, functional layer and anode layer, described cathode layer is multi-layer transparent electroconductive film, multi-layer transparent electroconductive film forms by cushioning matching layer, conductive layer and low work function layer, wherein, the material of described buffering matching layer is MeO, Me is Mg, Zn or Cd; The material of described conductive layer is Au; The material of described low work function layer is R
2o, R are Li, Na, K, Rb or Cs.
In described electroluminescent device, the thickness of described buffering matching layer is 50 ~ 150nm; The thickness of described conductive layer is 5 ~ 35nm; The thickness of described low work function layer is 1 ~ 10nm.
Further, in described electroluminescent device, the thickness of described buffering matching layer is 80nm; The thickness of described conductive layer is 25nm; The thickness of described low work function layer is 2nm.
The present invention as transparent conductive film by the film of preparation multilayer, can be utilized each layer to regulate the printing opacity of film, conduction and surface work function respectively, can keep good electric conductivity, work function can be made again to be significantly improved.Multi-layer transparent electroconductive film technique of the present invention is simple, and favorable reproducibility, is applicable to organic luminescent device OLED, the cathode layer of solar cell etc., and luminous efficiency can be made to be significantly improved.
Accompanying drawing explanation
Fig. 1 is the transmitted light spectrogram of multi-layer transparent electroconductive film prepared by the embodiment of the present invention 1.
Fig. 2 is the structural representation of electroluminescent device prepared by embodiment 1.
Fig. 3 is brightness and the voltage curve of electroluminescent device prepared by embodiment 1.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The embodiment of the present invention provides the present invention to propose a kind of multi-layer transparent electroconductive film, and it forms by cushioning matching layer, conductive layer and low work function layer, and wherein, the material of described buffering matching layer is MeO, Me is Mg, Zn or Cd; The material of described conductive layer is Au; The material of described low work function layer is R
2o, R are Li, Na, K, Rb or Cs.The thickness of described buffering matching layer is 50 ~ 150nm; The thickness of described conductive layer is 5 ~ 35nm; The thickness of described low work function layer is 1 ~ 10nm.
The preferred thickness of described buffering matching layer is 80nm; The preferred thickness of described conductive layer is 25nm; The preferred thickness of described low work function layer is 2nm.
Another goal of the invention of the present invention is the preparation method providing multi-layer transparent electroconductive film.
For above-mentioned purpose, the present invention proposes the preparation method that the present invention proposes a kind of multi-layer transparent electroconductive film, and it comprises the steps:
A () chooses MeO, Au and R respectively
2the powder of O, as target, loads in the vacuum cavity of filming equipment together with substrate;
B the vacuum degree of described vacuum cavity is evacuated to 1.0 × 10 by ()
-3pa ~ 1.0 × 10
-5pa, the spacing adjusting described substrate and described target is 35 ~ 95mm; Preferred vacuum degree in described cavity is 6.0 × 10
-4pa.The preferred distance of described substrate and described target is 60mm.
(c) over the substrate successively evaporation prepare MeO, Au and R
2o, described evaporation rate is 0.3 ~ 5nm/s.The evaporation rate of described MeO is 1 ~ 8nm/s, and the evaporation rate of described Au is 0.5 ~ 5nm/s, described R
2the evaporation rate of O is 0.3 ~ 3nm/s;
The preferred evaporation rate of described MeO is 3nm/s, and the preferred evaporation rate of described Au is 2nm/s, described R
2the preferred evaporation rate of O is 0.5nm/s;
Wherein, Me is Mg, Zn or Cd; R is Li, Na, K, Rb or Cs;
Another goal of the invention of the present invention is to provide a kind of electroluminescent device.
Below in conjunction with specific embodiment, the preparation method to above-mentioned multi-layer transparent electroconductive film and electroluminescent device thereof is described in detail.
Embodiment 1
The concrete preparation process of multi-layer transparent electroconductive film of the present embodiment is as follows:
1, successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning quartz substrate, and after drying up with high pure nitrogen, put into the vacuum cavity of filming equipment, load ZnO, Au and Li simultaneously
2cO
3powder is as target;
2, the distance of 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;
3, first evaporation ZnO, evaporation rate is 3nm/s, thickness 80nm; Then evaporation Au, evaporation rate is 2nm/s, thickness 25nm; Last evaporation Li
2o, evaporation rate is 0.5nm/s, and thickness is 2nm, namely obtains multi-layer transparent electroconductive film.
The multi-layer transparent electroconductive film square resistance obtained is 8 Ω/, and visible ray mean transmissivity is 85%, surface work function 2.7eV.
Refer to Fig. 1, Fig. 1 shows the transmitted light spectrogram of the multi-layer transparent electroconductive film of the embodiment of the present invention, and use ultraviolet-uisible spectrophotometer test, as can be seen from Figure 1, test wavelength is 300 ~ 900nm.Mean transmissivity in visible ray 470 ~ 790nm wave-length coverage reaches 89%.
Device embodiments
The electroluminescent device of the present embodiment prepared by the multi-layer transparent electroconductive film of Application Example 1.
As shown in Figure 2, this electroluminescent device comprises the glass substrate 301, cathode layer 302, functional layer 303 and the anode layer 304 that stack gradually.Wherein, the material of cathode layer 302 is be the ZnO (80nm) in embodiment 1, Au (25nm) and Li
2the multi-layer transparent electroconductive film that O (2nm) adulterates, the material of functional layer 303 is Alq
3, the material of anode layer 304 is ITO, AZO or IZO conducting film, from buying on the market.
The preparation method of electroluminescent device of application multi-layer transparent electroconductive film is: the multi-layer transparent electroconductive film in the cathode layer 302(the present embodiment in glass substrate 301 successively in evaporation the present embodiment), functional layer 303(material is Alq
3) and anode layer 304(ITO, AZO or IZO conducting film), obtain described electroluminescent device.
Wherein, the preparation method of multi-layer transparent electroconductive film is the described content of step 1 to step 3 of embodiment 1.
Refer to Fig. 3, Fig. 3 is the voltage of the electroluminescent device of the present embodiment 2 and electric current and brightness relationship figure, and curve 1 is voltage and current density relation curve in fig. 3, can find out electroluminescent device luminescence from 5.0V, curve 2 is voltage and brightness relationship curve, and high-high brightness is 130cd/m
2, show that the electroluminescent device of the present embodiment 2 has the good characteristics of luminescence.
Embodiment 2
The concrete preparation process of multi-layer transparent electroconductive film of the present embodiment is as follows:
1, successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning quartz substrate, and after drying up with high pure nitrogen, put into the vacuum cavity of filming equipment, load ZnO, Au and K simultaneously
2cO
3powder is as target;
2, the distance of target and substrate is set as 35mm; With mechanical pump and molecular pump, the vacuum degree of vacuum cavity is extracted into 1.0 × 10
-3pa;
3, first evaporation ZnO, evaporation rate is 1nm/s, thickness 50nm; Then evaporation Au, evaporation rate is 5nm/s, thickness 35nm; Last evaporation K
2o, evaporation rate is 0.3nm/s, and namely thickness 1nm obtains the multi-layer transparent electroconductive film of the present embodiment.The square resistance of this multi-layer transparent electroconductive film is 6 Ω/, and visible ray mean transmissivity is 82%, surface work function 3.1eV.
Embodiment 3
The concrete preparation process of multi-layer transparent electroconductive film of the present embodiment is as follows:
1, successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning quartz substrate, and after drying up with high pure nitrogen, put into the vacuum cavity of filming equipment, load ZnO, Au and Cs simultaneously
2cO
3powder is as target;
2, the distance of target and substrate is set as 90mm, with mechanical pump and molecular pump, the vacuum degree of vacuum cavity is extracted into 1.0 × 10
-5pa;
3, then evaporation ZnO, evaporation rate is 8nm/s, thickness 150nm; Evaporation Au again, evaporation rate is 0.5nm/s, thickness 5nm; Last evaporation Cs
2o, evaporation rate is 3nm/s, and thickness 10nm obtains the multi-layer transparent electroconductive film of the present embodiment.The square resistance of this multi-layer transparent electroconductive film is 30 Ω/, and visible ray mean transmissivity is 93%, surface work function 2.8eV.
Embodiment 4
The concrete preparation process of the present embodiment multi-layer transparent electroconductive film is as follows:
1, successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning quartz substrate, and after drying up with high pure nitrogen, put into the vacuum cavity of filming equipment, load MgO, Au and Li simultaneously
2cO
3powder is as target;
2, by MgO, Au and Li
2cO
3the distance of powder and substrate is set as 50mm, with mechanical pump and molecular pump, the vacuum degree of vacuum cavity is extracted into 6.0 × 10
-4pa;
3, then evaporation MgO, evaporation rate is 1nm/s, thickness 50nm, then evaporation Au, and evaporation rate is 5nm/s, thickness 35nm, last evaporation Li
2o, evaporation rate is 0.3nm/s, thickness 1nm, the sample obtained, and the square resistance of the multi-layer transparent electroconductive film obtained is 8 Ω/, and visible ray mean transmissivity is 89%, surface work function 2.8eV.
Embodiment 5
The concrete preparation process of multi-layer transparent electroconductive film of the present embodiment is as follows:
1, successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up with high pure nitrogen, put into the vacuum cavity of filming equipment, load MgO, Au and Na simultaneously
2cO
3powder is as target;
2, the distance of target and substrate is set as 35mm, with mechanical pump and molecular pump, the vacuum degree of vacuum cavity is extracted into 1.0 × 10
-3pa;
3, then evaporation MgO, evaporation rate is 3nm/s, thickness 80nm; Evaporation Au again, evaporation rate is 2nm/s, thickness 25nm, last evaporation Na
2o, evaporation rate is 0.5nm/s, and namely thickness 2nm obtains the multi-layer transparent electroconductive film of the present embodiment.The square resistance of this multi-layer transparent electroconductive film is 6 Ω/mouth, and visible ray mean transmissivity is 88%, surface work function 3.0eV.
Embodiment 6
The concrete preparation process of multi-layer transparent electroconductive film of the present embodiment is as follows:
1, successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up with high pure nitrogen, put into the vacuum cavity of filming equipment, what load also has MgO, Au and Rb simultaneously
2cO
3powder is as target;
2, the distance of target and substrate is set as 90mm, with mechanical pump and molecular pump, the vacuum degree of vacuum cavity is extracted into 1.0 × 10
-5pa;
3, then evaporation MgO, evaporation rate is 8nm/s, thickness 150nm; Evaporation Au again, evaporation rate is 0.5nm/s, thickness 5nm; Last evaporation Cs
2o, evaporation rate is 3nm/s, and namely film 10nm obtains the multi-layer transparent electroconductive film of the present embodiment.The square resistance of this multi-layer transparent electroconductive film is 30 Ω/mouth, and visible ray mean transmissivity is 93%, surface work function 2.8eV.
Embodiment 7
The concrete preparation process of multi-layer transparent electroconductive film of the present embodiment is as follows:
1, successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up with high pure nitrogen, put into the vacuum cavity of filming equipment, load CdO, Au and Na simultaneously
2cO
3powder is as target;
2, the distance of target and substrate is set as 50mm, with mechanical pump and molecular pump, the vacuum degree of vacuum cavity is extracted into 6.0 × 10
-4pa;
3, first evaporation CdO, evaporation rate is 1nm/s, thickness 50nm; Then evaporation Au, evaporation rate is 5nm/s, thickness 35nm; Last evaporation Na
2o, evaporation rate is 0.3nm/s, and namely film 1nm obtains the multi-layer transparent electroconductive film of the present embodiment.The square resistance of this multi-layer transparent electroconductive film is 8 Ω/mouth, and visible ray mean transmissivity is 85%, surface work function 2.7eV.
Embodiment 8
The concrete preparation process of multi-layer transparent electroconductive film of the present embodiment is as follows:
1, successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up with high pure nitrogen, put into the vacuum cavity of filming equipment, load CdO, Au and Rb simultaneously
2cO
3powder is as target;
2, the distance of target and substrate is set as 35mm, with mechanical pump and molecular pump, the vacuum degree of vacuum cavity is extracted into 1.0 × 10
-3pa;
3, first evaporation CdO, evaporation rate is 3nm/s, thickness 80nm; Then evaporation Au, evaporation rate is 2nm/s, thickness 25nm; Last evaporation Rb
2o, evaporation rate is 0.5nm/s, and namely thickness 2nm obtains the multi-layer transparent electroconductive film of the present embodiment.The square resistance of this multi-layer transparent electroconductive film is 6 Ω/mouth, and visible ray mean transmissivity is 86%, surface work function 3.0eV.
Embodiment 9
The present embodiment multi-layer transparent electroconductive film comprises Zn
0.85in
0.15o film and Cs
2o film, concrete preparation process is as follows:
1, successively by acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning quartz substrate, and dry up with high pure nitrogen, put into the vacuum cavity of filming equipment, load CdO, Au and Cs simultaneously
2cO
3powder is as target;
2, the distance of target and substrate is set as 90mm, with mechanical pump and molecular pump, the vacuum degree of vacuum cavity is extracted into 1.0 × 10
-5pa;
3, first evaporation CdO, evaporation rate is 8nm/s, thickness 150nm; Then evaporation Au, evaporation rate is 0.5nm/s, thickness 5nm; Last evaporation C
s2o, evaporation rate is 3nm/s, thickness 10nm.Namely the multi-layer transparent electroconductive film of the present embodiment is obtained.The square resistance of this multi-layer transparent electroconductive film is 30 Ω/mouth, and visible ray mean transmissivity is 90%, surface work function 2.9eV.
In above-described embodiment 2 to 9, the method that application multi-layer transparent electroconductive film prepares electroluminescent device is in the same manner as in Example 1, and just multi-layer transparent electroconductive film is replaced by the material in different embodiment, therefore does not repeat them here.
These are only better possible embodiments of the present invention, not limit the scope of the invention, all utilizations specification of the present invention and the change of the equivalent structure done by accompanying drawing content, be all included in protection scope of the present invention.
Claims (10)
1. a multi-layer transparent electroconductive film, is characterized in that, described multi-layer transparent electroconductive film forms by cushioning matching layer, conductive layer and low work function layer, and wherein, the material of described buffering matching layer is MeO, Me is Mg, Zn or Cd; The material of described conductive layer is Au; The material of described low work function layer is R
2o, R are Li, Na, K, Rb or Cs.
2. multi-layer transparent electroconductive film as claimed in claim 1, it is characterized in that, the thickness of described buffering matching layer is 50 ~ 150nm; The thickness of described conductive layer is 5 ~ 35nm; The thickness of described low work function layer is 1 ~ 10nm.
3. multi-layer transparent electroconductive film as claimed in claim 1, it is characterized in that, the thickness of described buffering matching layer is 80nm; The thickness of described conductive layer is 25nm; The thickness of described low work function layer is 2nm.
4. a preparation method for multi-layer transparent electroconductive film, is characterized in that, comprises the steps:
A () chooses MeO, Au and R respectively
2the powder of O, as target, loads in the vacuum cavity of filming equipment together with substrate;
B the vacuum degree of described vacuum cavity is evacuated to 1.0 × 10 by ()
-3pa ~ 1.0 × 10
-5pa, the spacing adjusting described substrate and described target is 35 ~ 95mm;
(c) over the substrate successively evaporation prepare MeO, Au and R
2o, described evaporation rate is 0.3 ~ 5nm/s;
Wherein, Me is Mg, Zn or Cd; R is Li, Na, K, Rb or Cs.
5. preparation method as claimed in claim 4, it is characterized in that, in described step (c), the evaporation rate of described MeO is 1 ~ 8nm/s, and the evaporation rate of described Au is 0.5 ~ 5nm/s, described R
2the evaporation rate of O is 0.3 ~ 3nm/s.
6. preparation method as claimed in claim 4, it is characterized in that, the thickness of described buffering matching layer is 50 ~ 150nm; The thickness of described conductive layer is 5 ~ 35nm; The thickness of described low work function layer is 1 ~ 10nm.
7. preparation method as claimed in claim 4, it is characterized in that, the thickness of described buffering matching layer is 80nm; The thickness of described conductive layer is 25nm; The thickness of described low work function layer is 2nm.
8. an electroluminescent device, it is straticulate structure, described straticulate structure is followed successively by glass substrate, cathode layer, functional layer and anode layer, it is characterized in that, described cathode layer is multi-layer transparent electroconductive film, and multi-layer transparent electroconductive film forms by cushioning matching layer, conductive layer and low work function layer, wherein, the material of described buffering matching layer is MeO, Me is Mg, Zn or Cd; The material of described conductive layer is Au; The material of described low work function layer is R
2o, R are Li, Na, K, Rb or Cs.
9. electroluminescent device as claimed in claim 8, it is characterized in that, the thickness of described buffering matching layer is 50 ~ 150nm; The thickness of described conductive layer is 5 ~ 35nm; The thickness of described low work function layer is 1 ~ 10nm.
10. electroluminescent device as claimed in claim 9, it is characterized in that, the thickness of described buffering matching layer is 80nm; The thickness of described conductive layer is 25nm; The thickness of described low work function layer is 2nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108281562A (en) * | 2017-01-05 | 2018-07-13 | 昆山工研院新型平板显示技术中心有限公司 | A kind of electrode and apply its organic electroluminescence device |
-
2013
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108281562A (en) * | 2017-01-05 | 2018-07-13 | 昆山工研院新型平板显示技术中心有限公司 | A kind of electrode and apply its organic electroluminescence device |
| US10957872B2 (en) | 2017-01-05 | 2021-03-23 | Kunshan New Flat Panel Display Technology Center Co. Ltd. | Electrode and organic electroluminescent device using same |
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