CN113421985A - Series OLED device and preparation method thereof - Google Patents

Series OLED device and preparation method thereof Download PDF

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CN113421985A
CN113421985A CN202110696237.8A CN202110696237A CN113421985A CN 113421985 A CN113421985 A CN 113421985A CN 202110696237 A CN202110696237 A CN 202110696237A CN 113421985 A CN113421985 A CN 113421985A
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layer
doping
moo
doped
substrate
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祝树炜
魏斌
严利民
宝庆云
谢孟坤
管新波
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Shanghai Jinghe Photoelectric Technology Co ltd
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
    • H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
    • H10K50/125—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers specially adapted for multicolour light emission, e.g. for emitting white light
    • H10K50/13—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers specially adapted for multicolour light emission, e.g. for emitting white light comprising stacked EL layers within one EL unit
    • H10K50/131—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers specially adapted for multicolour light emission, e.g. for emitting white light comprising stacked EL layers within one EL unit with spacer layers between the electroluminescent layers
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K2102/00—Constructional details relating to the organic devices covered by this subclass
    • H10K2102/301—Details of OLEDs
    • H10K2102/321—Inverted OLED, i.e. having cathode between substrate and anode

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Abstract

The invention relates to a series OLED device and a preparation method thereof, wherein the used connecting layers are a MoO3 doped layer and an Ag doped layer, and alkali metal ions do not exist, so that the failure of the device caused by the diffusion of the alkali metal ions into a light emitting layer is avoided, and the service life and the stability of the device are greatly improved. In addition, the invention adopts an inverted structure, and the electron transport material sensitive to water and oxygen is arranged below the device, so that the probability of contacting water and oxygen is reduced, the material failure of the device is slowed down, and the service life of the device is prolonged.

Description

Series OLED device and preparation method thereof
Technical Field
The invention relates to the technical field of organic light-emitting semiconductors, in particular to a series OLED device and a preparation method thereof.
Background
The existing OLED series technology connecting layer uses doping of alkali metal and organic matter, and alkali metal ions have a longer diffusion distance and can diffuse to a light-emitting layer to cause failure of a light-emitting layer material, so that the service life and stability of a device are influenced.
Therefore, there is a need in the art for a technical solution that effectively improves the performance and stability of the device while ensuring good carrier transport performance.
Disclosure of Invention
The invention aims to provide a series OLED device and a preparation method thereof, and solves the problems that the diffusion distance of alkali metal ions used in the prior series technology is long, and the service life and the stability of the device are influenced.
In order to achieve the purpose, the invention provides the following scheme:
a tandem OLED device comprising:
the light-emitting diode comprises a substrate layer, an electron injection layer, an electron transport layer, a light-emitting layer, a hole transport layer, a connecting layer and a metal electrode which are sequentially arranged from bottom to top;
the connecting layer is MoO3Doped layers and Ag doped layers.
A tandem OLED device comprising:
the light emitting diode comprises a substrate layer, an electron injection layer, an electron transport layer, a light emitting layer, a hole transport layer, a connecting layer, an electron transport layer, a light emitting layer, a hole transport layer, a second connecting layer and a metal electrode which are sequentially arranged from bottom to top;
the connecting layer is MoO3Doping layers and Ag doping layers;
the second connecting layer is MoO3And (5) doping the layers.
Optionally, the connecting layer is two layers;
one layer is MoO3Doping layer; and the other layer is an Ag doped layer.
Optionally, the MoO3The doping bodies of the doping layer and the Ag doping layer are as follows: one of NPB, BPhen, MCP and POT 2T.
Alternatively to this, the first and second parts may,
the MoO3The doping ratio of (A) is 20%;
the doping proportion of the Ag is 15%.
Alternatively to this, the first and second parts may,
the substrate layer is indium tin oxide;
the electron injection layer is BPhen doped with 15% Ag;
the electron transmission layer is one of B3PYMPM, TPBi and TMPYPB;
the light-emitting layer is DSA-ph doped ADN;
the hole transport layer is one of TCTA, PEDOT, PSS, TAPC and PVK;
the metal electrode is one of Al, Au, Ag and Cu.
Alternatively to this, the first and second parts may,
the thickness of the electron injection layer is 10 nm;
the thickness of the electron transport layer is 30 nm;
the thickness of the luminescent layer is 20 nm;
the thickness of the hole transport layer is 10 nm;
the thickness of the connecting layer is 50 nm; wherein MoO3The thickness of the doped layer is 40nm, and the thickness of the Ag doped layer is 10 nm;
the thickness of the metal electrode is 150 nm.
A method of making a tandem OLED device, the method comprising:
preparing a substrate layer;
sequentially evaporating materials of an electron injection layer, an electron transport layer, a light-emitting layer, a hole transport layer, a connecting layer and a metal electrode to the substrate layer; the connecting layer is MoO3Doped layers and Ag doped layers.
A method of making a tandem OLED device, the method comprising:
preparing a substrate layer;
sequentially evaporating materials of an electron injection layer, an electron transport layer, a light-emitting layer, a hole transport layer, a connecting layer, an electron transport layer, a light-emitting layer, a hole transport layer, a second connecting layer and a metal electrode onto the substrate layer; the connecting layer is MoO3Doping layers and Ag doping layers; the second connecting layer is MoO3And (5) doping the layers.
Optionally, the preparing the substrate layer specifically includes:
preparing an indium tin oxide substrate as a substrate layer;
putting the indium tin oxide substrate into a glass tank filled with deionized water, adding detergent powder and detergent, performing ultrasonic treatment for 90 minutes by using an ultrasonic machine, sequentially replacing the solution in the glass tank with deionized water, acetone and isopropanol, and performing ultrasonic treatment for 90 minutes respectively;
the indium tin oxide substrate was baked dry and UV treated.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
because the connecting layer used by the invention is MoO3The doping layer and the Ag doping layer do not have alkali metal ions, so that the failure of the device caused by the diffusion of the alkali metal ions into the light emitting layer is avoided, and the service life and the stability of the device are greatly improved. In addition, the invention adopts an inverted structure, and the electron transport material sensitive to water and oxygen is arranged below the device, so that the probability of contacting water and oxygen is reduced, the material failure of the device is slowed down, and the service life of the device is prolonged.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a schematic diagram of a conventional tandem OLED device according to an embodiment of the present invention.
Fig. 2 is an overall schematic view of a tandem OLED device according to a first embodiment of the present invention.
FIG. 3 is a schematic diagram of the composition of each layer of a tandem OLED device according to an embodiment of the present invention
Fig. 4 is an overall schematic diagram of a tandem OLED device according to a second embodiment of the present invention.
Fig. 5 is a schematic diagram illustrating the composition of each layer of a tandem OLED device according to a second embodiment of the present invention.
Fig. 6 is a current density and current efficiency characterization diagram of a series OLED device according to a second embodiment of the present invention.
Fig. 7 is a graph illustrating luminance and power density characteristics of a tandem OLED device according to a second embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
With current technology, the preparation of tandem structures is generally shown in the above figure, where the tie layer is formed using Alq 3: Li/NPB: FeCl3The preparation method comprises the following steps:
an ITO (indium tin oxide) is used as an anode of the device, a hole transport layer, a light emitting layer, an electron transport layer, a connecting layer, a hole transport layer, a light emitting layer and an electron transport layer are sequentially evaporated on the anode, and finally a metal electrode is evaporated to be used as a cathode, as shown in figure 1.
The invention aims to provide a series OLED device and a preparation method thereof, and solves the problems that the diffusion distance of alkali metal ions used in the prior series technology is long, and the service life and the stability of the device are influenced.
The invention provides a series structure based on an n-i-p-n type structure, which is suitable for an OLED device, a layer of n type doping is added on the basis of the traditional p-i-n type structure, and two Light-Emitting structures are connected in series through a novel connecting layer used by the invention, so that the performance and the stability of the device are effectively improved, and the problems that the existing device structure cannot ensure the stability of the OLED (Organic Light-Emitting Diode) device and the connecting layer cannot ensure the high performance of the device are solved, wherein i is a Light-Emitting layer emitter, n type doping majority is electrons, p type doping majority is holes, such as NPB: ag is n-type doped because it loses electrons therein to form silver ions, which become majority electrons, and is thus n-type doped.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
The first embodiment is as follows:
as shown in fig. 2, an embodiment of the present invention provides a tandem OLED device including:
the light-emitting diode comprises a substrate layer, an electron injection layer, an electron transport layer, a light-emitting layer, a hole transport layer, a connecting layer and a metal electrode which are sequentially arranged from bottom to top; the connecting layer is MoO3Doped layers and Ag doped layers.
As shown in fig. 3, in the present embodiment, the substrate layer is an ITO anode, the electron injection layer is a 15% metal-doped phenanthroline derivative, the light-emitting layer is a 5% light-emitting material-doped material, and the connection layer is a 20% metal-oxide-doped material and a 15% metal-doped phenanthroline derivative. The connecting layer is used for adjusting the balance of holes and electrons, so that the recombination efficiency of carriers is improved, and the performance of the device is improved.
Specifically, the connecting layer in this embodiment is two layers;
one layer is MoO3Doping layer; and the other layer is an Ag doped layer.
MoO3The doping bodies of the doping layer and the Ag doping layer are as follows: one of NPB, BPhen, MCP and POT 2T. In this embodiment, MoO is preferably used3Doped NPB and Ag doped BPhen.
Wherein, MoO3The doping ratio of (A) is 20%; the doping proportion of Ag is 15%.
As an alternative, the materials and thicknesses of the layers in this embodiment may be selected as follows:
the substrate layer is indium tin oxide;
the electron injection layer is BPhen doped with 15% Ag;
the electron transmission layer is one of B3PYMPM, TPBi and TMPYPB;
the light emitting layer is DSA-ph doped ADN;
the hole transport layer is one of TCTA, PEDOT, PSS, TAPC and PVK;
the metal electrode is one of Al, Au, Ag, and Cu.
The thickness of the electron injection layer is 10 nm;
the thickness of the electron transport layer is 30 nm;
the thickness of the light-emitting layer is 20 nm;
the thickness of the hole transport layer is 10 nm;
the thickness of the connecting layer is 50 nm; wherein MoO3The doped layer is 40nm, and the thickness of the Ag doped layer is 10 nm;
the thickness of the metal electrode was 150 nm.
Some of the terms of expertise in this example are defined as follows:
NPB: n, N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine;
b3 PYMPM: 4, 6-bis (3, 5-bis (3-pyridin) ylphenyl) -2-methylpyrimidine;
BPhen: 4, 7-diphenyl-1, 10-phenanthroline;
DSA-ph: 4,4' - [1, 4-phenylenedi- (1E) -2, 1-ethenediyl ] bis [ N, N-diphenylaniline ], a blue-light emitting material;
ADN: 9, 10-bis (2-naphthyl) anthracene;
TCTA: 4,4' -tris (carbazol-9-yl) triphenylamine.
The embodiment also provides a preparation method of the series OLED device, which comprises the following steps:
a1, preparing a substrate layer;
the method comprises the following specific steps:
preparing an indium tin oxide substrate as a substrate layer;
cleaning the substrate: and putting the indium tin oxide substrate into a glass tank filled with deionized water, adding detergent and detergent, performing ultrasonic treatment for 90 minutes by using an ultrasonic machine, sequentially replacing the solution in the glass tank with the deionized water, acetone and isopropanol, and performing ultrasonic treatment for 90 minutes respectively to complete cleaning of the substrate.
The indium tin oxide substrate was baked under a heating lamp and subjected to UV treatment for 15 minutes.
A2, sequentially mixingMaterials of the electron injection layer, the electron transport layer, the light-emitting layer, the hole transport layer, the connecting layer and the metal electrode are evaporated on the substrate layer; the connecting layer is MoO3Doped layers and Ag doped layers.
Specifically, a substrate is moved into a vacuum evaporation chamber, a material to be evaporated on the substrate is placed into an evaporation boat or a crucible of the evaporation chamber, the material is heated to a volatilization temperature in a current heating mode, and temperatures of evaporation sources with different evaporation rates are detected by a film thickness meter in an instrument and can be respectively controlled;
operating the instrument, vacuumizing the evaporation chamber to make the vacuum degree in the evaporation chamber reach 10-5And heating the crucible or the evaporation boat below Pa to make the material to be evaporated reach the evaporation temperature, and then evaporating the materials of the electron injection layer, the electron transport layer, the luminescent layer, the hole transport layer, the connecting layer and the metal electrode onto the substrate layer in sequence.
The preparation environment is kept at a vacuum degree of 10 during the preparation process-5Pa below; if only one material is in a layer, the material is heated to the volatilization temperature (different volatilization temperatures of different materials) by current, the volatilization rate of the material is detected by a film thickness meter, and the control is carried out
Figure BDA0003128532490000061
If one layer is doped with two materials, the two materials are heated and volatilized respectively, the volatilization rates are detected, and the doping proportion is adjusted according to the difference of the volatilization rates.
The connection layer used in the embodiment of the invention is MoO3The doping layer and the Ag doping layer do not have alkali metal ions, so that the failure of the device caused by the diffusion of the alkali metal ions into the light emitting layer is avoided, and the service life and the stability of the device are greatly improved. In addition, the invention adopts an inverted structure, and the electron transport material sensitive to water and oxygen is arranged below the device, so that the probability of contacting water and oxygen is reduced, the material failure of the device is slowed down, and the service life of the device is prolonged.
Example two:
as shown in fig. 4, an embodiment of the present invention provides a tandem OLED device including:
the light emitting diode comprises a substrate layer, an electron injection layer, an electron transport layer, a light emitting layer, a hole transport layer, a connecting layer, an electron transport layer, a light emitting layer, a hole transport layer, a second connecting layer and a metal electrode which are sequentially arranged from bottom to top;
the connecting layer is MoO3Doping layers and Ag doping layers;
the second connecting layer is MoO3And (5) doping the layers.
As shown in fig. 5, in this embodiment, the substrate layer is an ITO anode, the electron injection layer is a 15% metal-doped phenanthroline derivative, the light-emitting layer is a 5% light-emitting material-doped material, the connection layer is a 20% metal-oxide-doped material and a 15% metal-doped phenanthroline derivative, and the second connection layer is a 20% metal-oxide-doped material. The connecting layer is used for adjusting the balance of holes and electrons, so that the recombination efficiency of carriers is improved, and the performance of the device is improved.
It should be noted that the serial OLED device provided in this embodiment is a stacked device, please refer to fig. 5, the stacked layers may be multilayered within a certain range of layers, and if the layers are multilayered, the current efficiency, external quantum efficiency, and other properties of the device can be further improved, but if the layers are too high, the improvement may not be obvious due to too thick device.
Specifically, the connecting layer in this embodiment is two layers;
one layer is MoO3Doping layer; and the other layer is an Ag doped layer.
MoO3The doping bodies of the doping layer and the Ag doping layer are as follows: one of NPB, BPhen, MCP and POT 2T. In this embodiment, MoO is preferably used3Doped NPB and Ag doped BPhen.
Wherein, MoO3The doping ratio of (A) is 20%; the doping proportion of Ag is 15%.
As an alternative, the materials and thicknesses of the layers in this embodiment may be selected as follows:
the substrate layer is indium tin oxide;
the electron injection layer is BPhen doped with 15% Ag;
the electron transmission layer is one of B3PYMPM, TPBi and TMPYPB;
the light emitting layer is DSA-ph doped ADN;
the hole transport layer is one of TCTA, PEDOT, PSS, TAPC and PVK;
the metal electrode is one of Al, Au, Ag, and Cu.
The thickness of the electron injection layer is 10 nm;
the thickness of the electron transport layer is 30 nm;
the thickness of the light-emitting layer is 20 nm;
the thickness of the hole transport layer is 10 nm;
the thickness of the connecting layer is 50 nm; wherein MoO3The doped layer is 40nm, and the thickness of the Ag doped layer is 10 nm;
the thickness of the metal electrode was 150 nm.
The embodiment also provides a preparation method of the series OLED device, which comprises the following steps:
b1, preparing a substrate layer;
the method comprises the following specific steps:
preparing an indium tin oxide substrate as a substrate layer;
cleaning the substrate: and putting the indium tin oxide substrate into a glass tank filled with deionized water, adding detergent and detergent, performing ultrasonic treatment for 90 minutes by using an ultrasonic machine, sequentially replacing the solution in the glass tank with the deionized water, acetone and isopropanol, and performing ultrasonic treatment for 90 minutes respectively to complete cleaning of the substrate.
The indium tin oxide substrate was baked under a heating lamp and subjected to UV treatment for 15 minutes.
B2, sequentially evaporating materials of the electron injection layer, the electron transport layer, the light-emitting layer, the hole transport layer, the connecting layer, the electron transport layer, the light-emitting layer, the hole transport layer, the second connecting layer and the metal electrode to the substrate layer; the connecting layer is MoO3Doping layers and Ag doping layers; the second connecting layer is MoO3And (5) doping the layers.
Specifically, a substrate is moved into a vacuum evaporation chamber, a material to be evaporated on the substrate is placed into an evaporation boat or a crucible of the evaporation chamber, the material is heated to a volatilization temperature in a current heating mode, and temperatures of evaporation sources with different evaporation rates are detected by a film thickness meter in an instrument and can be respectively controlled;
operating the instrument, vacuumizing the evaporation chamber to make the vacuum degree in the evaporation chamber reach 10-5And heating the crucible or the evaporation boat below Pa to make the material to be evaporated reach the evaporation temperature, and then evaporating the materials of the electron injection layer, the electron transport layer, the luminescent layer, the hole transport layer, the connecting layer, the electron transport layer, the luminescent layer, the hole transport layer, the second connecting layer and the metal electrode onto the substrate layer in sequence.
The preparation environment is kept at a vacuum degree of 10 during the preparation process-5Pa below; if only one material is in a layer, the material is heated to the volatilization temperature (different volatilization temperatures of different materials) by current, the volatilization rate of the material is detected by a film thickness meter, and the control is carried out
Figure BDA0003128532490000081
If one layer is doped with two materials, the two materials are heated and volatilized respectively, the volatilization rates are detected, and the doping proportion is adjusted according to the difference of the volatilization rates.
Characterization of the tandem OLED devices provided in this example by a dc power supply, Keithley 2400Source Meter and a luminance spectrometer PR650 device manufactured by Photo Research are shown in fig. 6 and 7, and the characterization data are as follows:
device with a metal layer Film thickness of doped silver ion [ nm ]] Power onPressure [ V ]] Maximum current efficiency cd A-1] Maximum power efficiency lm w-1] Maximum external quantum efficiency [% ]]
Reference to 0 3.1 13.23 9.44 5.71
10nm 10 3.1 12.96 9.89 5.22
20nm 20 3.1 9.93 7.88 3.95
30nm 40 3.2 4.36 3.01 1.55
Laminate layer 10 5.8 27.91 11.26 11.18
As can be seen from the characterization results, the current efficiency of the stacked device, i.e., the serial OLED device provided in this embodiment, is improved by more than two times compared to that of a single-layer device, and the power efficiency and EQE (external quantum efficiency) are also significantly improved.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.

Claims (10)

1. A tandem OLED device, comprising:
the light-emitting diode comprises a substrate layer, an electron injection layer, an electron transport layer, a light-emitting layer, a hole transport layer, a connecting layer and a metal electrode which are sequentially arranged from bottom to top;
the connecting layer is MoO3Doped layers and Ag doped layers.
2. A tandem OLED device, comprising:
the light emitting diode comprises a substrate layer, an electron injection layer, an electron transport layer, a light emitting layer, a hole transport layer, a connecting layer, an electron transport layer, a light emitting layer, a hole transport layer, a second connecting layer and a metal electrode which are sequentially arranged from bottom to top;
the connecting layer is MoO3Doping layers and Ag doping layers;
the second connecting layer is MoO3And (5) doping the layers.
3. The tandem OLED device of claim 1 or 2, wherein the connecting layer is two layers;
one layer is MoO3Doping layer; and the other layer is an Ag doped layer.
4. The tandem OLED device of claim 1 or 2, wherein the MoO3The doping bodies of the doping layer and the Ag doping layer are as follows: one of NPB, BPhen, MCP and POT 2T.
5. The tandem OLED device according to claim 1 or 2,
the MoO3The doping ratio of (A) is 20%;
the doping proportion of the Ag is 15%.
6. The tandem OLED device according to claim 1 or 2,
the substrate layer is indium tin oxide;
the electron injection layer is BPhen doped with 15% Ag;
the electron transmission layer is one of B3PYMPM, TPBi and TMPYPB;
the light-emitting layer is DSA-ph doped ADN;
the hole transport layer is one of TCTA, PEDOT, PSS, TAPC and PVK;
the metal electrode is one of Al, Au, Ag and Cu.
7. The tandem OLED device according to claim 1 or 2,
the thickness of the electron injection layer is 10 nm;
the thickness of the electron transport layer is 30 nm;
the thickness of the luminescent layer is 20 nm;
the thickness of the hole transport layer is 10 nm;
the thickness of the connecting layer is 50 nm; wherein MoO3The thickness of the doped layer is 40nm, and the thickness of the Ag doped layer is 10 nm;
the thickness of the metal electrode is 150 nm.
8. A method of fabricating a tandem OLED device, the method comprising:
preparing a substrate layer;
sequentially evaporating materials of an electron injection layer, an electron transport layer, a light-emitting layer, a hole transport layer, a connecting layer and a metal electrode to the substrate layer; the connecting layer is MoO3Doped layers and Ag doped layers.
9. A method of fabricating a tandem OLED device, the method comprising:
preparing a substrate layer;
sequentially evaporating materials of an electron injection layer, an electron transport layer, a light-emitting layer, a hole transport layer, a connecting layer, an electron transport layer, a light-emitting layer, a hole transport layer, a second connecting layer and a metal electrode onto the substrate layer; the connecting layer is MoO3Doping layers and Ag doping layers; the second connecting layer is MoO3And (5) doping the layers.
10. The method for manufacturing a tandem OLED device according to claim 8 or 9, wherein the manufacturing of the substrate layer specifically includes:
preparing an indium tin oxide substrate as a substrate layer;
putting the indium tin oxide substrate into a glass tank filled with deionized water, adding detergent powder and detergent, performing ultrasonic treatment for 90 minutes by using an ultrasonic machine, sequentially replacing the solution in the glass tank with deionized water, acetone and isopropanol, and performing ultrasonic treatment for 90 minutes respectively;
the indium tin oxide substrate was baked dry and UV treated.
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