WO2019237479A1 - 一种电极及其制备方法和有机电致发光器件 - Google Patents

一种电极及其制备方法和有机电致发光器件 Download PDF

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Publication number
WO2019237479A1
WO2019237479A1 PCT/CN2018/099399 CN2018099399W WO2019237479A1 WO 2019237479 A1 WO2019237479 A1 WO 2019237479A1 CN 2018099399 W CN2018099399 W CN 2018099399W WO 2019237479 A1 WO2019237479 A1 WO 2019237479A1
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Prior art keywords
film
zinc oxide
electrode
indium zinc
substrate
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French (fr)
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木村徹
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Wuhan China Star Optoelectronics Semiconductor Display Technology Co Ltd
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Wuhan China Star Optoelectronics Semiconductor Display Technology Co Ltd
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Priority to US16/303,280 priority Critical patent/US20210226151A1/en
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
    • H10K59/80—Constructional details
    • H10K59/805—Electrodes
    • H10K59/8051—Anodes
    • H10K59/80517—Multilayers, e.g. transparent multilayers
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/20—Metallic material, boron or silicon on organic substrates
    • 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
    • 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
    • H10K50/80—Constructional details
    • H10K50/805—Electrodes
    • H10K50/81—Anodes
    • H10K50/816—Multilayers, e.g. transparent multilayers
    • 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
    • H10K50/80—Constructional details
    • H10K50/805—Electrodes
    • H10K50/82—Cathodes
    • H10K50/828—Transparent cathodes, e.g. comprising thin metal layers
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/06—Alloys based on silver
    • 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
    • H10K2102/351—Thickness
    • 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]
    • H10K50/14—Carrier transporting layers
    • H10K50/15—Hole transporting layers
    • 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]
    • H10K50/14—Carrier transporting layers
    • H10K50/16—Electron transporting layers
    • 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]
    • H10K50/17—Carrier injection layers
    • H10K50/171—Electron injection layers

Definitions

  • the present application relates to the field of display technology, and in particular, to an anode structure that can be used in an organic electroluminescent device, and a preparation method and application thereof.
  • OLED Organic Light-Emitting Diode
  • ITO Indium tin oxide
  • the organic electroluminescent device 1 includes an anode 12, an organic layer 14 and a cathode 16 formed on a substrate 10.
  • the organic layer 14 includes an electron injection layer 141, an electron transport layer 143, a light emitting layer 145, a hole transport layer 147, and a hole injection layer 149.
  • the anode 12 is an ITO / Ag / ITO three-layer conductive film composed of a high work function and high reflectivity ITO film and a metal film (usually silver, Ag), and the cathode 16 is Mg / Ag alloy of low work function metal magnesium and silver.
  • the conductive film composed of three layers of ITO / Ag / ITO needs to be wet-etched.
  • FIG. 2 illustrates a flowchart of preparing the anode of the organic electroluminescent device 1 described above.
  • microcrystalline ITO Micro-crystal The production of ITO, ⁇ C -ITO
  • the film formation of the first ITO film and the second ITO film is performed at low temperature (room temperature) to prevent Micro-crystallization of ITO. Since the etching rates of the ITO film and the Ag film are different, as shown in FIG.
  • over-etching is likely to occur when the first layer of ITO film is etched, and over-etching of the ITO film may cause the Ag film to be exposed, which may cause undesirable results such as sulfurization of the Ag film.
  • crystallization of ITO can improve the transmittance characteristics of the ITO film, as shown in FIG. 2, after the wet etching process, further annealing treatment (heat treatment) is required to crystallize the ITO film.
  • heat treatment annealing treatment
  • the crystallization of ITO will cause the ITO film surface to bulge (concavo-convex), and then produce submicron-level hemispherical protrusions on the Ag film surface (that is, the Hillock phenomenon of the Ag film), resulting in the destruction of the film As well as short circuit traces.
  • an ITO / Ag / ITO etching solution for AM-OLED display screens has been developed.
  • the special etching solution is mainly made of phosphoric acid, acetic acid, nitric acid, surfactants, additives and pure water by stirring, mixing and filtering.
  • the special etching solution is unstable in nature, and it is difficult to control the etching angle and the etching amount of the Ag film during the etching process, thereby affecting the repeatability of the etching effect.
  • the object of the present application is to provide an electrode and a method for preparing the same, which can be applied to OLED display technology or flexible OLED display technology.
  • the present application first provides an electrode composed of a first indium zinc oxide film, a metal film, and a second indium zinc oxide film that are sequentially stacked, wherein the metal film is made of an Ag alloy to make.
  • the thickness of the first indium zinc oxide film is 5 nm to 40 nm; the thickness of the metal film is 80 nm to 160 nm; the thickness of the second indium zinc oxide film is 5 nm ⁇ 40 nm.
  • the Ag alloy is a silver-palladium-copper alloy (Ag-Pd-Cu).
  • the present application further provides a method for preparing the above electrode, including the following steps: Step S1. Providing a film-forming substrate; Step S2. Forming a first indium-zinc oxide film with a thickness of 5 nm to 40 nm on the film-forming substrate Step S3. Forming a metal film with a thickness of 80 nm to 160 nm on the first indium zinc oxide film; and step S4. Forming a second film with a thickness of 5 nm to 40 nm on the metal film Indium zinc oxide film; wherein the metal film is made of an Ag alloy.
  • the film-forming substrate is a glass substrate, a polyimide substrate, or a film substrate.
  • the Ag alloy is a silver-palladium-copper alloy (Ag-Pd-Cu).
  • the first indium zinc oxide film, the metal film, and the second indium zinc oxide film are formed by a DC magnetron sputtering process.
  • the DC power is 2 kW to 8 kW, and the sputtering gas pressure is 0.2 Pa to 1.0 Pa.
  • the DC magnetron sputtering process can be performed by any known equipment.
  • the DC magnetron sputtering process is performed in a vacuum coating equipment.
  • the vacuum coating equipment is, for example but not limited to, a single coating equipment, a continuous coating equipment or an integrated coating equipment.
  • the DC magnetron sputtering process is completed in a film forming chamber in the vacuum coating equipment.
  • the vacuum degree in the film forming chamber is below 4 ⁇ 10 -5 Pa
  • the sputtering gas is an inert gas, such as, but not limited to, argon (Ar).
  • oxygen (O) may be added to the Ar gas. 2 ) or hydrogen (H 2 ), the volume percentage of the oxygen is controlled to be 0.1% to 5%, and the flow rate of the hydrogen is 1 to 10 standard milliliter / minute (sccm).
  • the DC magnetron sputtering process is performed using an indium zinc oxide target material, wherein the Zn content in the indium zinc oxide target material is 1 ⁇ 10wt%; and in step S3, the DC magnetron sputtering process is performed using a silver-palladium-copper alloy target.
  • a method for preparing an electrode includes the following steps: step S1. Providing a film-forming substrate; step S2. Performing a DC magnetron sputtering process using an indium zinc oxide target, A first indium-zinc oxide film having a thickness of 5 nm to 40 nm is formed on the film-forming substrate; step S3. A DC magnetron sputtering process using a silver-palladium-copper alloy target is performed on the first Forming an indium zinc oxide film with a thickness of 80 nm to 160 nm; and step S4.
  • the present application also provides an organic electroluminescent device, using the above electrode as an anode of the organic electroluminescent device.
  • Organic electroluminescence device using the above electrode as an anode of the organic electroluminescent device.
  • the organic electroluminescent device includes a substrate, and a first electrode, an organic layer, and a second electrode sequentially disposed on the substrate.
  • the first electrode is an anode
  • the second electrode is a cathode.
  • the organic layer includes an electron injection layer, an electron transport layer, a light emitting layer, a hole transport layer, and a hole injection layer which are disposed in this order.
  • the anode is composed of a first In-Zn-Oxide (IZO) film, a metal film (Ag-Pd-Cu, Ag-Pd-Cu, APC for short) and a second indium-zinc oxide film. Composition of IZO / APC / IZO conductive film.
  • the cathode is made of any known cathode material, such as a Mg / Ag alloy.
  • the organic layer may also include other functional layers, which are different according to the specific performance of different organic electroluminescent devices. The different composition of the organic layer does not affect the structure of the anode.
  • the present application also provides a display panel.
  • the display panel includes:
  • a substrate which is a glass substrate, a polyimide substrate, or a film substrate (film substrate);
  • An organic electroluminescent device layer said organic electroluminescent device layer being formed on said thin film transistor device layer;
  • the organic electroluminescent device layer includes a first electrode as an anode, an organic layer, and a second electrode as a cathode, and the first electrode is in contact with the drain of the thin film transistor device layer;
  • the first electrode is composed of a first indium zinc oxide film, a metal film, and a second indium zinc oxide film, which are sequentially stacked.
  • the metal film is made of an Ag alloy.
  • the thickness of the first indium zinc oxide film is 5 nm to 40 nm; the thickness of the metal film is 80 nm to 160 nm; the thickness of the second indium zinc oxide film 5 nm ⁇ 40 nm.
  • the Ag alloy is a silver-palladium-copper alloy (Ag-Pd-Cu).
  • Ag-Pd-Cu silver-palladium-copper alloy
  • the silver-palladium-copper alloy is a known and commercially available material.
  • the weight percentage of the silver element in the silver-palladium copper alloy ranges from 90% to 95%
  • the weight percentage of the palladium element ranges from 4% to 8%
  • the weight percentage of the copper element is about 1%.
  • the indium zinc oxide film is an amorphous film and the etching rate is fast, in the preparation process of the organic electroluminescent device using the electrode described in the present application, only an Ag alloy etching solution and equipment can be used, that is, The electrode can be wet-etched, so that the same etching solution can be used to complete the electrode etching on the same etching equipment, and the purpose of simplifying the OLED manufacturing process is achieved.
  • the indium zinc oxide film is an amorphous film, it has similar transmittance characteristics as crystalline ITO, so that the annealing process is not required during the manufacturing process of the electrode of the present application, thereby avoiding high temperatures during the annealing process. Hillock phenomenon of the Ag film caused by the reaction.
  • FIG. 1 is a schematic structural diagram of a conventional organic electroluminescent device
  • FIG. 2 is a flowchart of anode film formation and etching of a conventional organic electroluminescent device
  • FIG. 3 is a schematic structural diagram of an electrode according to an embodiment of the present application.
  • FIG. 5 is a schematic structural diagram of an organic electroluminescent device according to an embodiment of the present application.
  • FIG. 6 is a flowchart of film formation and etching of the electrode 3 of the organic electroluminescent device 5 shown in FIG. 5;
  • FIG. 7 is a schematic structural diagram of a display panel according to an embodiment of the present application.
  • the "first” or “lower” of the first feature may include the first and second features in direct contact, and may also include the first and second features. Not directly, but through another characteristic contact between them.
  • the first feature is “above”, “above”, and “above” the second feature, including that the first feature is directly above and obliquely above the second feature, or merely indicates that the first feature is higher in level than the second feature.
  • the first feature is “below”, “below”, and “below” of the second feature, including the fact that the first feature is directly below and obliquely below the second feature, or merely indicates that the first feature is less horizontal than the second feature.
  • an electrode 3 is provided. As shown in FIG. 3, the electrode 3 is composed of a first indium zinc oxide film 31, a metal film 32, and a second indium zinc oxide film 33 that are sequentially stacked.
  • the thickness of the first indium zinc oxide film 31 is 5 nm to 40 nm; the thickness of the metal film 32 is 80 nm to 160 nm; the thickness of the second indium zinc oxide film 31 is 5 nm to 40 nm.
  • the metal film 32 is made of Ag-Pd-Cu.
  • the silver-palladium-copper alloy is a known and commercially available material. Generally, the weight percentage of the silver element in the silver-palladium copper alloy ranges from 90% to 95%, the weight percentage of the palladium element ranges from 4% to 8%, and the weight percentage of the copper element is about 1%.
  • a method for preparing the foregoing electrode 3 including the following steps:
  • Step S1 A film-forming substrate is provided.
  • the film-forming substrate is a glass substrate, a polyimide substrate, or a film substrate. It can be understood that a number of steps are performed on the film-forming substrate.
  • the structure for example, may have an inorganic film layer, several film layers in a thin film transistor structure, or a complete thin film transistor and wiring have been formed. The specifics of the film layer to be formed in this process are different in the entire process flow. .
  • Step S2 The substrate obtained in step S1 is placed in a film forming chamber of a vacuum coating apparatus, and the vacuum degree in the film forming chamber is controlled to be 4 ⁇ 10 -5 Pa or less, and an indium zinc oxide target is used for direct current.
  • Step S3 Under the same vacuum as step S2, a DC magnetron sputtering process is performed using a silver-palladium-copper alloy target to form a metal with a thickness of 80 nm to 160 nm on the first indium zinc oxide film. Film; wherein the Zn content in the indium zinc oxide target is 1 to 10wt%;
  • Step S4 Under the same vacuum as step S2, a DC magnetron sputtering process is performed using an indium zinc oxide target to form a second indium zinc oxide with a thickness of 5 nm to 40 nm on the metal film.
  • a DC magnetron sputtering process is performed using an indium zinc oxide target to form a second indium zinc oxide with a thickness of 5 nm to 40 nm on the metal film.
  • the DC power is 2 kW to 8 kW
  • the sputtering gas is argon
  • the sputtering gas pressure is 0.2 Pa to 1 Pa.
  • the vacuum coating equipment is, for example but not limited to, a single coating equipment, a continuous coating equipment or an integrated coating equipment.
  • oxygen (O 2 ) or hydrogen (H 2 ) may be added to the Ar gas.
  • the volume percentage of the oxygen is controlled to be 0.1% to 5%, and the flow rate of the hydrogen is 1 to 10 standard milliliter / minute (sccm).
  • An organic electroluminescent device 5 is provided in this embodiment, as shown in FIG. 5.
  • the organic electroluminescent device 5 has a substrate 50.
  • the substrate 50 may be a glass substrate, a polyimide substrate, or a thin film substrate according to specific applications. It can be understood that A structure that has undergone several previous steps is formed on the film-forming substrate, for example, there may be an inorganic film layer, several film layers in a thin film transistor structure, or a complete thin film transistor and wiring have been formed, according to the process to be formed. The layers of the film in the whole process flow are different.
  • An organic electroluminescence device is provided on the substrate 50 with the electrode 3 as an anode, an organic layer 54 and a cathode 52 in this order.
  • the organic layer 54 of the organic electroluminescence device 5 has a structure known in the art, or other auxiliary function layers may be added according to actual application situations.
  • the organic layer 54 includes an electron injection layer 541, an electron transport layer 543, a light emitting layer 545, a hole transport layer 547, and a hole injection layer 549.
  • the cathode 52 is made of a metal having a lower work function such as lithium, magnesium, calcium, strontium, aluminum, indium, or an alloy thereof with copper, gold, and silver, such as, but not limited to, an AL, Mg / Ag alloy.
  • the cathode 52 may be an electrode layer formed alternately of a metal and a metal fluoride, such as, but not limited to, an electrode layer composed of a lithium fluoride and an Al layer sequentially stacked.
  • the cathode 52 may also be made of ITO or IZO.
  • the electron injection layer 541 may be made of, for example, but not limited to, one of graphene, carbon nanotubes, ZnO, TiO 2 , and Cs 2 CO 3 .
  • the electron transport layer 543 can be made of, for example, but not limited to, 4,7-diphenyl-1,10-phenanthroline (Bphen), 1,3,5-tris (N-phenylbenzimidazole-2- Based on benzene (TPBi), bath copper spirit (BCP), tris (8-hydroxyquinoline) aluminum (Alq3).
  • the hole-transporting layer 547 may be made of, for example, but not limited to, aromatic diamine compounds, aromatic triamine compounds, carbazole compounds, triphenylamine compounds, furan compounds, helical compounds, and polymer materials. Made of one of them.
  • FIG. 6 is a flowchart of film formation and etching of the electrode 3 of the organic electroluminescent device 5.
  • the electrode 3 can be performed using only an Ag alloy etching solution and equipment. Wet etching, so that the same etching solution is used to complete the etching of the electrode 3 on the same etching equipment, and the purpose of simplifying the OLED manufacturing process is achieved.
  • the indium zinc oxide film is an amorphous film, but it has similar transmittance characteristics as the crystallized ITO, an annealing process is not required in the process of the electrode 3, thereby avoiding the high temperature reaction caused by the annealing process. Hillock phenomenon of the Ag film.
  • a display panel 7 is provided in this embodiment, as shown in FIG. 7. As shown in FIG. 7, the display panel 7 includes:
  • a substrate 70 which is a glass substrate, a polyimide substrate, or a film substrate (film substrate);
  • the organic electroluminescent device layer includes the electrode 3 as an anode, an organic layer 741, and a second electrode 742 as a cathode.
  • the display panel 7 has a necessary structure of an OLED display panel known in the art.
  • the thin film transistor device layer 72 includes: a buffer layer 722 formed on the substrate 70, an active layer 723 formed on the buffer layer 722, and the active layer A gate insulating layer 724 on the layer 723, a gate layer 725 formed on the gate insulating layer 724, an insulating layer 726 formed on the gate layer 725, and a source formed on the insulating layer 726 An electrode and the drain 721, a flat layer 727 formed on the source and the drain 721, and a flat layer 727 formed.

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Abstract

本申请提供一种电极由依次层叠的一第一铟锌氧化物膜、一金属膜和一第二铟锌氧化物膜组成，其中，所述金属膜由Ag合金制成。所述第一铟锌氧化物膜的厚度为5 nm ~ 40 nm；所述金属膜的厚度为80 nm ~160 nm；所述第二铟锌氧化物膜的厚度为5 nm ~ 40 nm。该电极可以应用于OLED显示技术或柔性OLED显示技术中。

Description

一种电极及其制备方法和有机电致发光器件 技术领域
本申请涉及显示技术领域，特别涉及一种可用于有机电致发光器件的阳极结构及其制备方法和应用。
 背景技术
有机电致发光器件(Organic Light-Emitting Diode，OLED)因具有自发光、低能耗、宽视角、色彩丰富、快速响应及可制备柔性屏等诸多优异特性，已成为新一代的平面显示器技术。
铟锡氧化物(ITO)导电膜因具有低电阻率、高透光性、良好的高温稳定性等特点，以及制备和图形加工工艺简单等优点，被作为一种理想的透明电极材料而广泛应用于有机电致发光器件中。
请参见图1，图1所示的是目前广泛使用的有机电致发光器件。如图1所示的，所述有机电致发光器件1由形成于一基板10上的阳极12、有机层14和阴极16组成。其中，所述有机层14包括电子注入层141、电子传输层143、发光层145、空穴传输层147和空穴注入层149。通常，所述阳极12为由高功函高反射率的ITO膜与金属膜(通常为银，Ag)所组成的ITO/Ag/ITO三层叠加的导电膜，而所述阴极16则为为低功函的金属镁与银的Mg/Ag合金。
在上述有机电致发光器件1的制备过程中，为了制备所需要的电极图形，需要对所述由ITO/Ag/ITO三层叠加的导电膜进行湿蚀刻。
 技术问题
请参见图2，图2所示的是上述有机电致发光器件1的阳极制备流程图。由于在湿蚀刻过程中，微结晶化ITO(Micro-crystal ITO, μC -ITO)的产生会引起ITO残渣问题，因而在如图2所示的制备过程中，第一ITO膜及第二ITO膜的成膜是在低温（室温）下进行的，以防止ITO的微结晶化。由于ITO膜与Ag膜的蚀刻率不同，因而如图2所示的，在完成第一ITO膜成膜、Ag膜成膜、第二ITO膜成膜后，需要选用不同的蚀刻液依次对第一ITO膜、Ag膜和第二ITO膜进行湿蚀，从而造成制备工艺的复杂化。
此外，在蚀刻第一层ITO膜时容易发生过蚀刻，而该ITO膜的过蚀刻会引起Ag膜露出，进而造成Ag膜硫化等不良结果。
再者，由于结晶化ITO可以提高ITO膜的穿透率特性，因而如图2所示的，在湿蚀刻处理之后，需要进一步进行退火处理（热处理），以使ITO膜结晶化。然而，在退火处理中，ITO的结晶化会使得ITO膜表面发生隆起（凹凸），进而在Ag膜表面产生亚微米级的半球状突起物（即Ag膜发生Hillock现象），从而导致膜的破坏以及走线短路等问题。
为解决上述ITO膜与Ag膜需要分步蚀刻的问题，目前已开发一种AM-OLED显示屏专用的ITO/Ag/ITO蚀刻液。该专用蚀刻液主要由磷酸、醋酸、硝酸、表面活性剂、添加剂和纯水经搅拌混匀过滤制得。然而，该专用蚀刻液性质不稳定，且在蚀刻过程中难以控制蚀刻角度及Ag膜的蚀刻量，从而影响蚀刻效果的可重复性。
因此，有必要提供一种新的电极材料及应用该电极材料的有机电致发光器件，以克服上述缺陷。
 技术解决方案
本申请的目的在于提供一种电极及其制备方法，该电极可以应用于OLED显示技术或柔性OLED显示技术中。
为了达到上述目的，本申请首先提供一种电极，由依次层叠的一第一铟锌氧化物膜、一金属膜和一第二铟锌氧化物膜组成，其中，所述金属膜由Ag合金制成。
在一实施例中，所述第一铟锌氧化物膜的厚度为5 nm ~ 40 nm；所述金属膜的厚度为80 nm ~160 nm；所述第二铟锌氧化物膜的厚度为5 nm ~ 40 nm。
在一实施例中，所述Ag合金为银钯铜合金（Ag-Pd-Cu）。
本申请还提供上述电极的制备方法，包括以下步骤：步骤S1. 提供一成膜基板；步骤S2.在所述成膜基板上形成一厚度为5 nm ~ 40 nm的第一铟锌氧化物膜；步骤S3.在所述第一铟锌氧化物膜上形成一厚度为80 nm ~160 nm的金属膜；以及，步骤S4.在所述金属膜上形成一厚度为5 nm ~ 40 nm第二铟锌氧化物膜；其中，所述金属膜由Ag合金制成。
在一实施例中，在所述步骤S1中，所述成膜基板为玻璃基板、聚酰亚胺基板或薄膜基板(film基板)。
在一实施例中，所述Ag合金为银钯铜合金（Ag-Pd-Cu）。
在一实施例中，以直流磁控溅镀制程形成所述第一铟锌氧化物膜、所述金属膜及所述第二铟锌氧化物膜。
在一实施例中，在所述直流磁控溅镀制程中，直流功率为2 kW ~ 8 kW，溅射气压为0.2 Pa ~1.0 Pa。
本领域技术人员可以理解的是，可以以任何已知的设备进行所述直流磁控溅镀制程。例如，在一实施例中，在一真空镀膜设备中进行所述直流磁控溅镀制程。所述真空镀膜设备例如但不限于，单体镀膜设备、连续式镀膜设备或集成式镀膜设备。
在一实施例中，在所述真空镀膜设备中的成膜腔室内完成所述直流磁控溅镀制程。所述成膜腔室内的真空度在4×10 -5 Pa以下，溅射气体采用惰性气体，例如但不限于氩气(Ar)。并且，可选地，在步骤S2及所述步骤S4的形成所述第一铟锌氧化物膜及所述第二铟锌氧化物膜的过程中，可以在所述Ar气体中添加氧气(O 2)或氢气(H 2)，控制所述氧气的体积百分比为0.1% ~ 5%，所述氢气的流量为1 ~ 10标准毫升/分(sccm)。
在一实施例中，在所述步骤S2和所述步骤S4中，使用铟锌氧化物靶材进行所述直流磁控溅镀制程，其中，所述铟锌氧化物靶材中Zn含量为1 ~ 10wt%；而在所述步骤S3中，使用银钯铜合金靶材进行所述直流磁控溅镀制程。
因此，在本申请一具体实施例中，提供一种电极的制备方法，包括以下步骤：步骤S1. 提供一成膜基板；步骤S2. 使用铟锌氧化物靶材进行直流磁控溅镀制程，以在所述成膜基板上形成一厚度为5 nm ~ 40 nm的第一铟锌氧化物膜；步骤S3. 使用银钯铜合金靶材进行直流磁控溅镀制程，以在所述第一铟锌氧化物膜形成一厚度为80 nm ~160 nm的金属膜；以及，步骤S4. 使用铟锌氧化物靶材进行直流磁控溅镀制程，以在所述金属膜上形成一厚度为5 nm ~ 40 nm的第二铟锌氧化物膜；其中，在所述直流磁控溅镀制程中，直流功率为2 kW ~ 8 kW，溅射气体为氩气，溅射气压为0.2 Pa ~1 Pa；并且，所述步骤S1至步骤S4在一真空镀膜设备的成膜腔室内进行，所述成膜腔室内的真空度在4×10 -5 Pa以下。
本申请还提供一种有机电致发光器件，将上述电极用为所述有机电致发光器件的阳极。有机电致发光器件有机电致发光器件
在本申请一实施例中，所述有机电致发光器件包括一基板，以及依次设置在所述基板上的一第一电极、一有机层和一第二电极。其中，所述第一电极为阳极，所述第二电极为阴极。所述有机层包括依次设置的一电子注入层、一电子传输层、一发光层、一空穴传输层和一空穴注入层。所述阳极为一由第一铟锌氧化物(In-Zn-Oxide，简称IZO)膜、金属膜(银钯铜合金，Ag-Pd-Cu，简称APC)和第二铟锌氧化物膜所组成的IZO/APC/IZO导电膜。所述阴极则由任意已知的阴极材料制成，例如Mg/Ag合金。所述有机层也可以包括其他功能层，具体根据不同有机电致发光器件的具体性能不同而不同。所述有机层的不同组成不影响所述阳极的结构。
此外，本申请还提供一种显示面板，所述显示面板包括：
一基板，所述基板为一玻璃基板、一聚酰亚胺基板或薄膜基板(film基板)；
一薄膜晶体管器件层，所述薄膜晶体管器件层形成于所述基板上，并具有一漏极；以及，
一有机电致发光器件层，所述有机电致发光器件层形成于所述薄膜晶体管器件层上；
其中，所述有机电致发光器件层包括作为阳极的一第一电极、一有机层和作为阴极的一第二电极，所述第一电极与所述薄膜晶体管器件层的所述漏极接触；并且，
所述第一电极由依次层叠的一第一铟锌氧化物膜、一金属膜和一第二铟锌氧化物膜组成，其中，所述金属膜由Ag合金制成。
在本申请一实施例中，所述第一铟锌氧化物膜的厚度为5 nm ~ 40 nm；所述金属膜的厚度为80 nm ~160 nm；所述第二铟锌氧化物膜的厚度为5 nm ~ 40 nm。
在本申请一实施例中，所述Ag合金为银钯铜合金（Ag-Pd-Cu）。本领域技术人员可以理解的是，所述银钯铜合金为一已知且市售的材料。通常，银钯铜合金中银元素的重量百分比范围为90%~95%，钯元素的重量百分比范围为4%-~8%，铜元素的重量百分比为1%左右。
 有益效果
在本申请中，由于铟锌氧化物膜是非结晶膜，蚀刻率很快，因而在使用本申请所述电极的有机电致发光器件的制备工艺中，可以仅使用Ag合金的蚀刻液及设备即可对所述电极进行湿蚀刻，进而实现在同一蚀刻设备上使用同一蚀刻液完成所述电极的蚀刻，达到简化OLED制备工艺的目的。此外，尽管铟锌氧化物膜是非结晶膜，但其具有与结晶化ITO相似的穿透率特性，因而本申请的所述电极的制造过程中不需要进行退火处理，从而避免了退火处理中高温反应造成的所述Ag膜的Hillock现象。
 附图说明
为了更清楚地说明本发明实施例中的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1是一现有有机电致发光器件的结构示意图；
图2是一现有有机电致发光器件的阳极成膜及蚀刻流程图；
图3是根据本申请一实施例的一电极的结构示意图；
图4是根据本申请一实施例的所述电极的制备流程图；
图5是根据本申请一实施例的一有机电致发光器件的结构示意图；
图6是图5所示有机电致发光器件5的电极3的成膜及蚀刻流程图；
图7是根据本申请一实施例的一显示面板的结构示意图。
 本发明的最佳实施方式
下面详细描述本发明的实施方式，所述实施方式的示例在附图中示出，其中自始至终相同或类似的标号表示相同或类似的元件或具有相同或类似功能的元件。下面通过参考附图描述的实施方式是示例性的，仅用于解释本发明，而不能理解为对本发明的限制。
在本发明中，除非另有明确的规定和限定，第一特征在第二特征之“上”或之“下”可以包括第一和第二特征直接接触，也可以包括第一和第二特征不是直接接触而是通过它们之间的另外的特征接触。而且，第一特征在第二特征“之上”、“上方”和“上面”包括第一特征在第二特征正上方和斜上方，或仅仅表示第一特征水平高度高于第二特征。第一特征在第二特征“之下”、“下方”和“下面”包括第一特征在第二特征正下方和斜下方，或仅仅表示第一特征水平高度小于第二特征。
下文的公开提供了许多不同的实施方式或例子用来实现本发明的不同结构。为了简化本发明的公开，下文中对特定例子的部件和设置进行描述。当然，它们仅仅为示例，并且目的不在于限制本发明。此外，本发明可以在不同例子中重复参考数字和/或参考字母，这种重复是为了简化和清楚的目的，其本身不指示所讨论各种实施方式和/或设置之间的关系。此外，本发明提供了的各种特定的工艺和材料的例子，但是本领域普通技术人员可以意识到其他工艺的应用和/或其他材料的使用。
在本实施例中，提供一电极3。如图3所示的，所述电极3由依次层叠的一第一铟锌氧化物膜31、一金属膜32和一第二铟锌氧化物膜33组成。
所述第一铟锌氧化物膜31的厚度为5 nm ~ 40 nm；所述金属膜32的厚度为80 nm ~160 nm；所述第二铟锌氧化物膜31的厚度为5 nm ~ 40 nm。所述金属膜32由银钯铜合金（Ag-Pd-Cu）制成。所述银钯铜合金为一已知且市售的材料。通常，银钯铜合金中银元素的重量百分比范围为90%~95%，钯元素的重量百分比范围为4%-~8%，铜元素的重量百分比为1%左右。
如图4所示的，在本实施例中提供上述电极3的制备方法，包括以下步骤：
步骤S1. 提供一成膜基板，所述成膜基板为一玻璃基板、一聚酰亚胺基板或薄膜基板(film基板)；可以理解的是，在成膜基板上形成有经过前序若干工序的结构，例如可能有无机膜层、薄膜晶体管结构中的若干膜层或者已经形成完整的薄膜晶体管及走线，具体根据本工艺所对应要形成的膜层在整个工艺流程中的环节不同而不同。
步骤S2. 将步骤S1获得的基板置于一真空镀膜设备的成膜腔室内，并控制所述成膜腔室内的真空度在4×10 -5 Pa以下，使用铟锌氧化物靶材进行直流磁控溅镀制程，以在所述成膜基板上形成一厚度为5 nm ~ 40 nm的第一铟锌氧化物膜；
步骤S3. 在与步骤S2相同的真空度下，使用银钯铜合金靶材进行直流磁控溅镀制程，以在所述第一铟锌氧化物膜形成一厚度为80 nm ~160 nm的金属膜；其中，所述铟锌氧化物靶材中Zn含量为1 ~ 10wt%；
步骤S4. 在与步骤S2相同的真空度下，使用铟锌氧化物靶材进行直流磁控溅镀制程，以在所述金属膜上形成一厚度为5 nm ~ 40 nm的第二铟锌氧化物膜；
其中，在所述直流磁控溅镀制程中，直流功率为2 kW ~ 8 kW，溅射气体为氩气，溅射气压为0.2 Pa ~1 Pa。
所述真空镀膜设备例如但不限于，单体镀膜设备、连续式镀膜设备或集成式镀膜设备。
在步骤S2及所述步骤S4的形成所述第一铟锌氧化物膜及所述第二铟锌氧化物膜的过程中，可以在Ar气体中添加氧气(O 2)或氢气(H 2)，控制所述氧气的体积百分比为0.1% ~ 5%，所述氢气的流量为1 ~ 10标准毫升/分(sccm)。
本发明的实施方式
实施例1. 有机电致发光器件
在本实施例中提供一有机电致发光器件5，请参见图5所示。
如图5所示的，所述有机电致发光器件5具有一基板50，所述基板50可以依据具体应用而选择一玻璃基板、一聚酰亚胺基板或一薄膜基板；可以理解的是，在成膜基板上形成有经过前序若干工序的结构，例如可能有无机膜层、薄膜晶体管结构中的若干膜层或者已经形成完整的薄膜晶体管及走线，具体根据本工艺所对应要形成的膜层在整个工艺流程中的环节不同而不同。在所述基板50上依次设置作为阳极的所述电极3、一有机层54和阴极52有机电致发光器件。
所述有机电致发光器件5的所述有机层54具有本领域已知的结构，或者还可以依据实际应用情况增加其他辅助功能层。例如，如图5所示的，所述有机层54包括一电子注入层541、一电子传输层543、一发光层545、一空穴传输层547和一空穴注入层549。
本领域技术人员可以理解的是，上述每一层结构所采用的材料均为本领域已知的，且这些材料的具体选择不影响本申请技术方案的实施及技术效果的获得。
所述阴极52采用锂、镁、钙、锶、铝、铟等功函数较低的金属或它们与铜、金、银的合金制成，例如但不限于，AL、Mg/Ag合金。或者，所述阴极52也可以是一金属与金属氟化物交替形成的电极层，例如但不限于，一由依次层叠的氟化锂及Al层组成的电极层。当然，所述阴极52也可以是由ITO或IZO制成。
所述电子注入层541可以由例如但不限于，石墨烯、碳纳米管、ZnO、TiO 2、Cs 2CO 3中的一种制成。
所述电子传输层543可以由例如但不限于，4,7-二苯基-1,10-菲罗啉(Bphen)、1,3,5-三(N-苯基苯并咪唑-2-基)苯(TPBi)、浴铜灵(BCP)、三(8-羟基喹啉)铝(Alq3)中的一种制成。
所述空穴传输层547可以由例如但不限于，芳香族二胺类化合物、芳香族三胺类化合物、咔唑类化合物、三苯胺类化合物、呋喃类化合物、螺形结构化合物、聚合物材料中的一种制成。
请参见图6，图6是所述有机电致发光器件5的所述电极3的成膜及蚀刻流程图。与图2相比，由于本实施例的所述电极3中的铟锌氧化物膜是非结晶膜，蚀刻率很快，因而可以仅使用Ag合金的蚀刻液及设备即可对所述电极3进行湿蚀刻，进而实现在同一蚀刻设备上使用同一蚀刻液完成所述电极3的蚀刻，达到简化OLED制备工艺的目的。此外，由于铟锌氧化物膜是非结晶膜，但其具有与结晶化ITO相似的穿透率特性，因而在所述电极3的制程中不需要进行退火处理，从而避免了退火处理中高温反应造成的所述Ag膜的Hillock现象。
实施例2. 显示面板
进一步地，在本实施例中还提供一种显示面板7，请参见图7所示。如图7所示的，所述显示面板7包括：
一基板70，所述基板70为一玻璃基板、一聚酰亚胺基板或薄膜基板(film基板)；
一薄膜晶体管器件层72，形成于所述基板70上，并具有一漏极721；以及，
一有机电致发光器件层74，形成于所述薄膜晶体管器件层72上；
其中，所述有机电致发光器件层包括作为阳极的所述电极3、一有机层741和作为阴极的一第二电极742，所述电极3与所述薄膜晶体管器件层72的所述漏极721接触。
本领域技术人员可以理解的是，所述显示面板7具有本领域已知的OLED显示面板的必要结构。例如，如图7所示的，所述薄膜晶体管器件层72包括：形成于所述基板70上的缓冲层722、形成于所述缓冲层722上的有源层723、形成于所述有源层723上的栅极绝缘层724、形成于所述栅极绝缘层724上的栅极层725、形成于所述栅极层725上的绝缘层726，形成于所述绝缘层726上的源极和所述漏极721、形成于所述源极和所述漏极721上的平坦层727和形成于所述平坦层727。
本申请已由上述相关实施例加以描述，然而上述实施例仅为实施本申请的范例。必需指出的是，已公开的实施例并未限制本申请的范围。相反地，包含于权利要求书的精神及范围的修改及均等设置均包括于本申请的范围内。

Claims (10)

  1. 一种用于有机电致发光器件的电极，所述有机电致发光器件由形成于一基板上的阳极、有机层和阴极组成，其中，所述电极由依次层叠的一第一铟锌氧化物膜、一金属膜和一第二铟锌氧化物膜组成，其中，所述金属膜由Ag合金制成。
  2. 如权利要求1所述的用于有机电致发光器件的电极，其中，所述第一铟锌氧化物膜的厚度为5 nm ~ 40 nm；所述金属膜的厚度为80 nm ~160 nm；所述第二铟锌氧化物膜的厚度为5 nm ~ 40 nm。
  3. 如权利要求1所述的用于有机电致发光器件的电极，其中，所述Ag合金为银钯铜合金。
  4. 一种用于有机电致发光器件的电极的制备方法，包括以下步骤：
    提供一成膜基板；
    在所述成膜基板上形成一厚度为5 nm ~ 40 nm的一第一铟锌氧化物膜；
    在所述第一铟锌氧化物膜上形成一厚度为80 nm ~160 nm的金属膜；以及，
    在所述金属膜上形成一厚度为5 nm ~ 40 nm第二铟锌氧化物膜；
    其中，所述金属膜由Ag合金制成。
  5. 如权利要求4所述的制备方法，其中，所述成膜基板为玻璃基板、聚酰亚胺基板或薄膜基板。
  6. 如权利要求4所述的制备方法，其中，所述Ag合金为银钯铜合金。
  7. 如权利要求4所述的制备方法，其中，以直流磁控溅镀制程形成所述第一铟锌氧化物膜、所述金属膜及所述第二铟锌氧化物膜。
  8. 如权利要求7所述的制备方法，其中，在所述直流磁控溅镀制程中，直流功率为2 kW ~ 8 kW，溅射气压为0.2 Pa ~1 Pa。
  9. 一种有机电致发光器件，包括形成于一基板上的一阳极、一有机层和一阴极，其中，如权利要求1所述的电极作为所述阳极。
  10. 如权利要求9所述的有机电致发光器件，其中，所述有机层包括依次设置的一电子注入层、一电子传输层、一发光层、一空穴传输层和一空穴注入层。
PCT/CN2018/099399 2018-06-13 2018-08-08 一种电极及其制备方法和有机电致发光器件 Ceased WO2019237479A1 (zh)

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