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WO2025051117A1 - Électrode transparente traitée en solution hautement stable faisant appel à un réseau de nanofils métalliques et des polymères - Google Patents

Électrode transparente traitée en solution hautement stable faisant appel à un réseau de nanofils métalliques et des polymères Download PDF

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Publication number
WO2025051117A1
WO2025051117A1 PCT/CN2024/116575 CN2024116575W WO2025051117A1 WO 2025051117 A1 WO2025051117 A1 WO 2025051117A1 CN 2024116575 W CN2024116575 W CN 2024116575W WO 2025051117 A1 WO2025051117 A1 WO 2025051117A1
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WO
WIPO (PCT)
Prior art keywords
polymer
layer
metallic
network
transparent electrode
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PCT/CN2024/116575
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English (en)
Inventor
Chik Ho Choy
Jiawei ZHENG
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University of Hong Kong HKU
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University of Hong Kong HKU
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F71/00—Manufacture or treatment of devices covered by this subclass
    • H10F71/138—Manufacture of transparent electrodes, e.g. transparent conductive oxides [TCO] or indium tin oxide [ITO] electrodes
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/20—Electrodes
    • H10F77/244—Electrodes made of transparent conductive layers, e.g. transparent conductive oxide [TCO] layers

Definitions

  • the present invention generally relates to a process for transparent electrodes. More specifically, the present invention relates to highly stable solution-processed transparent electrodes based on a metal nanowire network and polymers.
  • Transparent conductive electrodes are essential in modern industries, such as displays, solar cells, and detectors. Generally, high transmittance, high conductivity, and high stability are imperative requirements for TCEs. Tin-doped Indium Oxide (ITO) is currently the mainstream choice. However, the lack of storage of indium, high cost, and complicated deposition process would restrict its application in the near future. Metallic nanowire transparent conductive network, as an indium-free electrode material, with its superior photoelectric properties and mechanical flexibility, has attracted more and more attention from scientific research and industry.
  • nanowire (NW) networks have emerged in light-emitting diodes, solar cells, touch panels, flexible sensors, transparent heaters, and electromagnetic shielding and shows great potential as TCEs.
  • ITO the low manufacturing cost, easy-fabricating process, and great flexibility make Ag-NW suitable for large-scale and flexible applications.
  • TCEs the compatibility with other layers in the multi-layered device structure is essential.
  • the polymer post-treatment process of the present invention is to resolve the below two problems present in the field of the Ag nanowire network based top transparent electrode system.
  • the stability of the metallic network is considerably improved by polymer posttreatment.
  • the degradation mechanism of the metallic nanowires involves atomic diffusion of metal atoms or clusters under various activations. After compositing with polymer, the functional groups of polymers with linear, branched, or cross-linked structures strongly anchor the metal atoms and makes the diffusion barrier much higher than the reference. Thus, the thermal, electrical, and mechanical stabilities of nanowire networks significantly improved.
  • polymer interacted nanowire-based electrodes show better chemical stability against water/moisture, oxygen, or other environmental conditions than the controlled metal nanowire electrodes, resulting in improved chemical stability of the composite electrode.
  • a method of integrating a solution-processed transparent electrode based on a metallic nanowire network and polymers includes forming at least one metallic network on an underlying substrate via a solution process comprising a plurality of metal nanowires and a plurality of junctions where the metal nanowires meet; forming a gap filling layer on the metallic network to form a complex of metallic network and polymer; and drying the complex of metallic network and polymer, in which the metallic network and polymer are connected to each other at least by chemical bonding.
  • a transparent electrode based on a metallic nanowire network and polymer includes a plurality of metal oxide nanoparticles, at least one metal nanowire, and an anchoring polymer layer.
  • the metal oxide nanoparticles form a metal oxide layer.
  • the metal nanowire is positioned on the metal oxide layer.
  • the anchoring polymer layer connects to the metal nanowire and the metal oxide layer to form at least one junction point therebetween via chemical bonding of nitrogen.
  • Simple solution process and low cost a simple alcohol-based coating process for Ag nanowires, which avoids high energy consumption during the manufacturing process.
  • High transmittance of electrode the average transmittance of Ag networks is improved. especially in red region of visible light and the near-infrared region.
  • Green process low temperature, atmosphere condition, and non-toxic process.
  • FIG. 1 illustrates the angled SEM image and schematic diagram of the Ag nanowire network lying on the zinc oxide (ZnO) nanoparticles layer with PEI treatment according to some embodiments of the present invention
  • FIG. 2 illustrate performances of related devices according to some embodiments of the present invention, in which the section (a) shows current-voltage characteristics for ITO/ZnO NP/AgNW-based transparent conductive electrodes; and the section (b) shows the transmittance spectra of glass/ITO, glass/ITO/PEDOT: PSS, and ZnO/AgNW without and with PEI coatings;
  • FIG. 3 illustrate performances of related devices, in which the section (a) is the thermal stability of AgNW networks without and with PEI-10 treatment; the section (b) is the electrical stability of the AgNW networks without and with PEI-10 treatment at 5 V, and the inset diagram is the measured device structure of glass/ITO/ZnONP/AgNW/PEI-10; the section (c) is the storage stability of AgNW and AgNW/PEI-10 at 85 °C and 85%RH; and the section (d) is the chemical stability of AgNW and AgNW/PEI-10 immersed in 10 wt%polystyrene sulfonate solution; and the section (e) is the bending stability of AgNW network without and with PEI-10 treatment on 5 um cPI flexible substrate, and the bending radius is less than 2 mm; and the section (f) is the normalized current of the AgNW networks without and with PEI-10 treatment after around 10000 bending cycles;
  • FIG. 4 illustrate performances of related devices, in which the section (a) is the thermal stability of AgNW networks with PEI, PAA, PAA+PEI, and PAA+MEG treatments; the section (b) is the bending stability of the AgNW network with PEI, PAA, PAA+PEI, and PAA+MEG treatments on 5 um cPI flexible substrate, and the bending radius is less than 2 mm; and
  • FIG. 5 shows the schematic diagram of the formation process of the AgNW/polymer complex network.
  • a novel approach is provided, which can simultaneously improve the interfacial contact and electrode stabilities, such that a high-quality top transparent electrode can be manufactured by establishing silver nanowire composite with functional polymers via a facile solution process.
  • a method of integrating a solution-processed transparent electrode based on a metallic nanowire network and polymers including: step (a) : forming at least one metallic network on an underlying substrate via a solution process comprising a plurality of metal nanowires and a plurality of junctions where the metal nanowires meet (e.g., the first step of FIG. 5) ; step (b) : forming a gap filling layer on the metallic network to form a complex of metallic network and polymer (e.g., the second step of FIG. 5 or the second step in combination with the third step of FIG. 5) ; and step (c) : drying the complex of metallic network and polymer.
  • At least after the step (b) at least one adhesive force is created between the gap filling layer and the metallic network (i.e., metal nanowire network) via chemical bonding (e.g. nitrogen) for adhesion.
  • the metallic network i.e., metal nanowire network
  • chemical bonding e.g. nitrogen
  • adhesive force is created between the gap filling layer and the metal oxide nanoparticle film via chemical bonding (e.g. nitrogen) for adhesion as well.
  • contacts and adhesive forces among the underlying substrate, the metallic network, and the gap filling layer are enhanced via the chemical bonding.
  • a hybrid film including the metal nanowire network, and the metal oxide nanoparticle film is formed and obtained, which can be defined as a layer-by-layer structure.
  • the forming the gap filling layer is performed by forming a polymer film on the metallic network. More precisely, the polymer includes amine-based or acid-based, or sulfide-based polymer that has plentiful groups. In various embodiments, the polymer includes polyethylenimine (PEI) , poly (propylene imine) (PPI) , polyamidoamine (PAMAM) , Poly (acrylic acid) (PAA) , polystyrene sulfonate (PSS) , or combinations thereof. In one embodiment, the gap filling layer is formed at least using polymers containing nitrogen (amine) , such as polyethylenimine (PEI) .
  • PEI polyethylenimine
  • the forming the gap filling layer is performed by forming two layers of materials and then cross-linking the materials on the metallic network (e.g., the second step in combination with the third step of FIG. 5) .
  • the gap filling layer can include cross-linking materials combined with two materials, an anchor polymer and a cross-linker.
  • the anchor polymer includes polyethylenimine (PEI) , poly (propylene imine) (PPI) , polyamidoamine (PAMAM) , Poly (acrylic acid) (PAA) , polystyrene sulfonate (PSS) , or combinations thereof.
  • the cross-linker is polymer or monomer, including polyethylenimine (PEI) , poly (propylene imine) (PPI) , polyamidoamine (PAMAM) , Poly (acrylic acid) (PAA) , polystyrene sulfonate (PSS) , ethylene glycol (EG) , Oxalic acid, or combinations thereof.
  • PEI polyethylenimine
  • PPI poly (propylene imine)
  • PAMAM polyamidoamine
  • PAA acrylic acid
  • PSS polystyrene sulfonate
  • EG ethylene glycol
  • Oxalic acid Oxalic acid
  • the step of the cross-linking the materials on the metallic network is achieved by a cross-linking process, which is conducted by thermal annealing at a range of 50-150°C, or using UV treatment, or using cross-linking agent such as Sodium citrate and periodate potassium (KIO 4 ) , etc.
  • a cross-linking process which is conducted by thermal annealing at a range of 50-150°C, or using UV treatment, or using cross-linking agent such as Sodium citrate and periodate potassium (KIO 4 ) , etc.
  • the underlying substrate is a preparation substrate or target substrate.
  • the preparation substrate may be a silicon wafer, glass, etc.
  • the target substrate is a metal oxide film such as zinc oxide (ZnO) , titanium oxide (TiO 2 ) , tin oxide (SnO 2 ) , nickel oxide (NiO) , indium tin oxide (ITO) , aluminum oxide (Al 2 O 3 ) , or combinations thereof.
  • the preparation substrate is not limited to be composed only one metal; for example, in one embodiments, two or more different metal oxide compounds are applied to the preparation substrate.
  • At least one metallic nanowire of the metal nanowires includes silver, gold, platinum, aluminum, palladium, or combinations thereof.
  • the step of the forming the metallic network onto the underlying substrate includes: preparing the metallic nanowire in form of the solution; and forming the metallic network using spin coating, drop casting, spray coating, or blade coating techniques onto the underlying substrate.
  • a solvent for the metal nanowire includes ethanol, methanol, isopropanol, ethylene glycol, glycerin, or a mixture thereof.
  • the step of the forming the gap filling layer on the metallic network involves using polymer and includes: preparing the polymer in form of solution, in which a solution concentration of the polymer is in a range of 1-20 mg/mL; and coating the metallic network with the polymer in form of solution using spin coating, drop casting, spray coating, or blade coating techniques, so as to form a conductive polymer thin film.
  • a solvent of the polymer is ethanol, methanol, isopropanol, ethylene glycol, Glycerin, or a mixture thereof.
  • solution deposition techniques such as spin-coating, blade coating, inkjet printing, and Mayer rod coating, so one or more of these methods can be used for forming one target layer/film over a base (e.g., preparation substrate) .
  • the drying the complex of metallic network and polymer is processed under a temperature in a range of 70-150°C for about 10 minutes.
  • the complex of metallic network and polymer can serve as a conductive film which can realize a sheet resistance of lower than 20 ⁇ /sq, as well as achieving an average transmittance in the visible region over 50%.
  • the complex of metallic network and polymer can serve as a conductive film which can sustain a temperature of over 250 °C or a voltage over 10V.
  • the complex of metallic network and polymer can serve as a conductive film which can keep over 90%of its conductivity after 10000 bending cycles with a bending radius lower than 2 mm.
  • the silver nanowire (AgNW) /Polyethylenimine (PEI) results can be applied to describe the invention.
  • FIG. 1 illustrates the angled SEM image and schematic diagram of the Ag nanowire network lying on the zinc oxide (ZnO) nanoparticles layer with PEI treatment according to some embodiments of the present invention.
  • the illustration of FIG. 1 shows that the PEI can well cover the AgNW and fill the gap between top electrode-AgNW and underneath layer-ZnO, which can reduce the contact defects at the interface.
  • the PEI can connect to both the AgNW and the underlying ZnO layer via chemical bonding, (such as through nitrogen-containing functional groups) for adhesion.
  • a transparent electrode 100 based on a metallic nanowire network and polymer includes: a plurality of metal oxide nanoparticles forming a metal oxide layer 110; at least one metal nanowire 120 positioned on the metal oxide layer 110; and an anchoring polymer layer 130 connecting to the metal oxide layer 110 and the metal nanowire 120 to form at least one junction point (e.g., the circle nodes) therebetween via nitrogen.
  • the connection points for the junction are achieved with chemical bonding, enhancing contacts and adhesive forces between the metal oxide layer 110 and the anchoring polymer layer 130 and between the metal nanowire 120 and the anchoring polymer layer 130.
  • the mentioned chemical bonding of nitrogen for adhesion is a concept different than applying Van-der-Waals forces and/or other electrostatic interactions and/or capillary forces.
  • the anchoring polymer layer 130 extends from the metal oxide layer 110 to the metal nanowire 120 (which can be further illustrated in FIG. 5) .
  • the transparent electrode further includes a cross-linking layer 132 covering the metal nanowire 120 and the anchoring polymer layer 130.
  • the metal nanowire 120 is enclosed by the anchoring polymer layer 130 in combination with the cross-linking layer 132.
  • an entirety of the metal nanowire 120 can be protected by the anchoring polymer layer 130 in combination with the cross-linking layer 132.
  • the anchoring polymer layer 130 in combination with the cross-linking layer 132 serves as a complex of polymer conformally covering the metal nanowire 120 along a surface of the metal oxide layer 110. Therefore, the formed transparent electrode structure will exhibit fluctuations on the surface thereof.
  • the cross-linking layer 132 is a transparent or translucent solid that is formed/disposed over the metal oxide layer 110 and surrounds the areas where the metal nanowire 120 and the anchoring polymer layer 130 are located.
  • the cross-linking layer 132 can have a fixed contour/profile, thereby allowing the volume and shape of the transparent electrode 100 to remain roughly constant.
  • the anchoring polymer layer 130 acts as a gap-filling layer alone.
  • the complex of polymer resulting from the anchoring polymer layer 130 and the cross-linking layer 132 acts as a gap-filling layer collectively.
  • the metal oxide layer 110 is a zinc oxide nano-particle (ZnONP) layer; the metal oxide layer 110 is not limited to ZnO.
  • the metal oxide layer 110 is a layer formed by metal nano-particles titanium oxide (TiO 2 ) , tin oxide (SnO 2 ) , nickel oxide (NiO) , indium tin oxide (ITO) , aluminum oxide (Al 2 O 3 ) , or combinations thereof.
  • the anchoring polymer layer 130 is a polymer containing nitrogen (amine) , such as nitrogen-containing amine polymers or polyethylenimine (PEI) .
  • the transparent electrode 100 with such structure can be defined as a layer-by-layer structure.
  • FIG. 2 illustrate performances of related devices according to some embodiments of the present invention, in which the section (a) shows current-voltage characteristics for ITO/ZnO NP/AgNW-based transparent conductive electrodes; and the section (b) shows the transmittance spectra of glass/ITO, glass/ITO/PEDOT: PSS, and ZnO/AgNW without and with PEI coatings.
  • the current-voltage characteristics of the device with a structure of ITO/ZnO NP/AgNW-based TCEs have been measured to analyze the interfacial conductivity between ZnONP and AgNWs, as shown in the section (a) of FIG. 2.
  • the conductivity improves, indicating better contact at the interface.
  • PEI can fill the gap between ZnO and AgNW to achieve better contact and interfacial conductivity.
  • the transmittance and reflectance spectra use glasses as baselines are measured as shown in the section (b) of FIG. 2.
  • FIG. 3 illustrate performances of related devices, in which the section (a) is the thermal stability of AgNW networks without and with PEI-10 treatment; the section (b) is the electrical stability of the AgNW networks without and with PEI-10 treatment at 5 V, and the inset diagram is the measured device structure of glass/ITO/ZnONP/AgNW/PEI-10; the section (c) is the storage stability of AgNW and AgNW/PEI-10 at 85 °C and 85%RH; and the section (d) is the chemical stability of AgNW and AgNW/PEI-10 immersed in 10 wt%polystyrene sulfonate solution; and the section (e) is the bending stability of AgNW network without and with PEI-10 treatment on 5 um cPI flexible substrate, and the bending radius is less than 2 mm; and the section (f) is the normalized current of the AgNW networks without and with PEI-10 treatment after around 10000 bending cycles.
  • the section (a) is the thermal stability of
  • double-layer polymers can further improve the stabilities of AgNW electrodes.
  • Polyacrylic acid (PAA) which has abundant acid groups along with its chain, is chosen to cooperate with PEI to exhibit the improved stabilities of AgNW networks.
  • Figure 4 shows the thermal stability and mechanical stability of AgNW networks with PEI, PAA, PAA+PEI, and PAA+Mono Ethylene Glycol (MEG) .
  • PAA Compared with PEI, PAA demonstrates better stability, contributed by the stronger interaction between polymer and Ag.
  • PAA cooperated with PEI and MEG both exhibit better performance than pure PAA ones.
  • the atomic anchoring effect of polymer on the Ag surface prevents the surface Ag atom from diffusion during thermal annealing and mechanical bending, resulting in enhanced stability of the AgNW network.
  • the deposition of second layer materials on the network is aimed to cross-link with the first layer, which is expected to enhance structural stability.
  • Cross-linked polymers can sustain higher strain and lead to a superior performance of AgNW stability than single polymers, which is proved by FIG. 4. Astonishingly, the AgNW networks with PAA/PEI or PAA/MEG show negligible degradation after 18000 bending cycles with a bending radius of 2 mm.
  • FIG. 4 illustrate performances of related devices, in which the section (a) is the thermal stability of AgNW networks with PEI, PAA, PAA+PEI, and PAA+MEG treatments; the section (b) is the bending stability of the AgNW network with PEI, PAA, PAA+PEI, and PAA+MEG treatments on 5 um cPI flexible substrate, and the bending radius is less than 2 mm.
  • FIG. 5 shows the schematic diagram of the formation process of the AgNW/polymer complex network.
  • the formation process of the AgNW/polymer complex network is conducted with solution processed deposition methods, as shown in FIG. 5.
  • the first layer polymer is recognized as an ‘anchor polymer’ , which can strongly interact with Ag.
  • the second layer material could be a monomer or polymer which is employed as a ‘cross-linker’ .

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Abstract

L'invention concerne un procédé d'intégration d'une électrode transparente traitée en solution faisant appel à un réseau de nanofils métalliques et des polymères. Le procédé comprend la formation d'au moins un réseau métallique sur un substrat sous-jacent par l'intermédiaire d'un traitement en solution, comprenant une pluralité de nanofils métalliques et une pluralité de jonctions où les nanofils métalliques se rencontrent ; la formation d'une couche de remplissage d'interstice sur le réseau métallique pour former un complexe de réseau métallique et de polymère ; et le séchage du complexe de réseau métallique et de polymère, le réseau métallique et le polymère étant reliés l'un à l'autre au moins par liaison chimique.
PCT/CN2024/116575 2023-09-08 2024-09-03 Électrode transparente traitée en solution hautement stable faisant appel à un réseau de nanofils métalliques et des polymères Pending WO2025051117A1 (fr)

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US202363581282P 2023-09-08 2023-09-08
US63/581,282 2023-09-08

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100197068A1 (en) * 2008-10-30 2010-08-05 Hak Fei Poon Hybrid Transparent Conductive Electrode
US20120132930A1 (en) * 2010-08-07 2012-05-31 Michael Eugene Young Device components with surface-embedded additives and related manufacturing methods
KR20140066014A (ko) * 2012-11-22 2014-05-30 한국과학기술원 금속 나노선과 전도성 폴리머를 포함하는 투명 전극 및 그 제조방법
US20150359105A1 (en) * 2014-06-06 2015-12-10 Iinnova Dynamics, Inc. Patterned transparent conductors and related compositions and manufacturing methods
US20180358144A1 (en) * 2017-06-12 2018-12-13 Samsung Display Co., Ltd. Metal nanowire electrode and manufacturing method of the same

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100197068A1 (en) * 2008-10-30 2010-08-05 Hak Fei Poon Hybrid Transparent Conductive Electrode
US20120132930A1 (en) * 2010-08-07 2012-05-31 Michael Eugene Young Device components with surface-embedded additives and related manufacturing methods
KR20140066014A (ko) * 2012-11-22 2014-05-30 한국과학기술원 금속 나노선과 전도성 폴리머를 포함하는 투명 전극 및 그 제조방법
US20150359105A1 (en) * 2014-06-06 2015-12-10 Iinnova Dynamics, Inc. Patterned transparent conductors and related compositions and manufacturing methods
US20180358144A1 (en) * 2017-06-12 2018-12-13 Samsung Display Co., Ltd. Metal nanowire electrode and manufacturing method of the same

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