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WO2012055397A1 - Revêtement composite métallique présentant une transmissivité optique élevée dans le spectre visible - Google Patents

Revêtement composite métallique présentant une transmissivité optique élevée dans le spectre visible Download PDF

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Publication number
WO2012055397A1
WO2012055397A1 PCT/DE2011/001902 DE2011001902W WO2012055397A1 WO 2012055397 A1 WO2012055397 A1 WO 2012055397A1 DE 2011001902 W DE2011001902 W DE 2011001902W WO 2012055397 A1 WO2012055397 A1 WO 2012055397A1
Authority
WO
WIPO (PCT)
Prior art keywords
silver
composite
coating according
film
metal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/DE2011/001902
Other languages
German (de)
English (en)
Inventor
Mady Elbahri
Franz Faupel
Venkata Sai Kiran Chakravadhanula
Mehdi Keshavarz Hedayati
Thomas Strunskus
Vladimir Zaporojtchenko
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Christian Albrechts Universitaet Kiel
Original Assignee
Christian Albrechts Universitaet Kiel
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Christian Albrechts Universitaet Kiel filed Critical Christian Albrechts Universitaet Kiel
Publication of WO2012055397A1 publication Critical patent/WO2012055397A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025—Metallic sublayers
    • 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
    • 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
    • C23C14/12—Organic material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/14—Conductive material dispersed in non-conductive inorganic material
    • H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • 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
    • H10K50/85—Arrangements for extracting light from the devices
    • H10K50/854—Arrangements for extracting light from the devices comprising scattering means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • 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
    • H10K2102/331—Nanoparticles used in non-emissive layers, e.g. in packaging layer

Definitions

  • the invention relates to a visible-light-transmissive, electrically conductive coating for solar cells, MEMS, organic light-emitting diodes (OLED) or the like.
  • the invention particularly relates to transparent electrodes.
  • ITO indium tin oxide
  • VIS optical visual
  • NIR near-infrared
  • ITO indium tin oxide
  • ITO indium tin oxide
  • ITO indium
  • metal oxides such as ITO are brittle and tend to break under deformation, which can locally increase electrical resistance and also expose the substrate to atmospheric moisture and atmospheric oxygen.
  • An option for the replacement of ITO is quite the coating of the substrates with thin metal films, especially with precious metal films. Such films are already available from film
  • VIS transparency is to be referred to below in the sense that a VIS-transparent coating transmits at least 50% of the irradiated light intensity at least in partial regions of the VIS spectrum.
  • a coating according to the preamble of claim 1 is known for example from EP 2 287 939 AI.
  • Periodic arrays of similar nanometal particles in a dielectric matrix are generally candidates for so-called negative index materials (NIM). These are given a negative refractive index in accordance with their curious properties, in particular the unusual refraction of light and the amplification of evanescent fields.
  • LHM left-handed materials
  • the coating of the present invention is a double layer of a metal film not thicker than 30 nm and a composite film disposed on or under the metal film not thicker than 70 nm.
  • the composite film is made of a dielectric (nonconductive) matrix material having randomly distributed, electrically embedded therein conductive nanoparticles.
  • the degree of filling F of the composite film is between 3% and 15%.
  • Filling degree F is the volume fraction of the composite that the nanoparticles occupy.
  • a fill level of F - 50% means that the combined volume of all nanoparticles is just half the composite volume.
  • the metal film consists of gold, silver or copper.
  • gold and silver inherently have a comparatively high transmissivity in the range of the VIS spectrum.
  • the metal film may also be formed from common materials such as aluminum, iron (steel) or an alloy (eg silver-gold or nickel-titanium, shape memory metal).
  • the electrically conductive nanoparticles must exhibit metallic behavior, in particular the ability to plasma resonance. This is certainly the case if the nanoparticles are formed from element metals, ie element metal or alloy particles. But there are also about carbon nanotubes in question, which are known as good conductors.
  • the nanoparticles preferably consist of the precious metals gold or silver.
  • the nanoparticles do not have to be monodisperse. They should not have a regular arrangement, but a random distribution in the composite. In particular, it is sufficient to use particle distributions resulting from in situ generation of the particles during composite coating by a PVD process. Most preferably, the composites are formed by vacuum co-deposition of matrix material and metal on the metal film or substrate (see, e.g., DE 103 16 379 B4 and works cited therein).
  • the matrix material may be a dielectric metal oxide (e.g., S1O2) or a nonconductive organic plastic (e.g., PMMA, PTFE).
  • S1O2 dielectric metal oxide
  • PMMA polymethyl methacrylate
  • PTFE nonconductive organic plastic
  • the choice of matrix material is not essential to the effect of the invention, but rather, this choice is based on the coating process and on the requirements to be met by the coated substrate. For example, one will rather coat a flexible substrate with a flexible matrix, especially a polymer. Rigid solar cells, e.g. On the other hand, one would rather be equipped with a glass-like matrix, as exposed to highly variable environmental conditions (especially temperatures).
  • the double layer according to the invention is a layer up to 100 nm thick. It must be supported by a substrate to maintain its integrity, with either the metal film or the composite film directly on the substrate. When it comes to the electrical contacting of the substrate, it will be convenient to arrange the metal film on the substrate and the composite film on the metal film.
  • the reflectivity of both sides of the bilayer can be measured with one of the two sides illuminated by the substrate.
  • the double layer according to the invention is preferably characterized in that the wavelength-dependent reflectivities of both flat sides each have a local minimum with respect to ⁇ in the VIS spectral range (in this case specifically: 400-750 nm), for example at ⁇ for the metal film side and ⁇ for the composite side, wherein the Positions of these minima of depend on the degree of filling F of the composite.
  • a double layer with optimum transmissivity for given layer thicknesses of the metal film Dmet and the composite layer Dcomp is one whose degree of filling is minimized by the difference ⁇ -
  • the extent to which et and ⁇ approach or even bring to coincidence, can be determined by a series of experiments in the double layers with predetermined Dmet and Dcomp and varying degree of filling 0.03 ⁇ F ⁇ 0.15 arranged in the VIS spectrum highly transparent substrate and hereafter measured in terms of their reflectivities from both sides.
  • the degree of filling Fopt which leads to minimal ⁇ is then known for the specific choice of material (metal film, matrix, nanoparticles) and can be used to coat any substrates with this configuration.
  • the transmissi vity of double layers of a metal film of thickness Dmet ⁇ 30 nm and a composite layer of thickness Dcomp ⁇ 70 nm with degree of filling Fopt according to the above criterion is higher than the transmissivity of the metal film of thickness Dmet alone in wide areas of the VIS spectrum.
  • the transmissivity depends only weakly on the angle of incidence of the light against the surface normal and practically not on the azimuth angle (rotation about the surface normal).
  • the omnidirectional same transmission behavior is attributable to the random distribution of the nanoparticles.
  • FIG. 1 reflectivities of double layers with different degrees of filling taken from the composite side;
  • FIG. 2 shows positions of the local minima of the reflectivities for different filling levels of the double layer and taken in each case for the metal film and the composite film sides;
  • FIG. 3 Transmissivities of the bilayers of FIG. 1.
  • FIG. 4 transmissivity of a double layer according to the invention when light is incident at different angles
  • FIG. Fig. 5 Transmissivity of a silver film with and without a composite layer
  • FIG. 6 Improvement of the transmissivity of an Au / Ag alloy film through the composite layer.
  • Exemplary embodiments are double layers of noble metal films (gold, silver, gold-silver alloy) and composite layers with a matrix of Teflon® (PTFE, polytetrafluoroethylene) in which nanoparticles of elemental silver are embedded. All exemplary embodiments are produced by magnetron sputtering of precious metal on glass and subsequent vacuum codeposition of silver and Teflon vapor on the noble metal films. The silver vapor forms silver nanoparticles on condensation, and the Teflon vapor, which is actually composed of radical polymer fragments, re-crosslinks to the matrix of composite films.
  • the deposition rates can be determined independently with quartz microbalances. In particular, by controlling the deposition rates, the degree of filling of a composite film can be adjusted. He then remains unchanged over the film thickness.
  • the films are checked with a profilometer and the film thicknesses are measured.
  • degrees of filling are determined separately by means of energy-dispersive X-ray spectroscopy (EDX).
  • EDX energy-dispersive X-ray spectroscopy
  • FIG. 1 shows the reflectivities of the composite side (normal incidence) of double layers of 25 nm gold film and 20 nm silver / PTFE composite for the wavelength range 300-800 nm.
  • the double layers presented in FIG. 1 differ only by the set ones Degrees of filling ((a) 7%, (b) 13%, (c) 17%, (d) 23%).
  • a monotonic increase in the reflectivity with the degree of filling can be recognized, with the local minima of the reflectivity curves in the range 550-600 nm also shifting monotonically toward larger wavelengths.
  • the bilayers are arranged on VIS-transparent substrates such that the gold film is between substrate and composite.
  • the reflectivities of the gold film can be measured, which are also dependent on the degree of filling of the composite.
  • the transmissivity is always above 70% in the measurements shown in the range 500-750 nm, showing only weak dependence on the angle of incidence and practically none of the sample rotation.
  • the composite increases the transmissivity by almost 30% without significant dependence on the wavelength in the VIS spectrum.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Optics & Photonics (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Laminated Bodies (AREA)

Abstract

L'invention concerne un revêtement électroconducteur transparent à la lumière visible, comportant une couche double constituée d'un film métallique d'une épaisseur comprise entre 10 et 30 nm et d'une couche composite dont l'épaisseur ne dépasse pas 70 nm comprenant un matériau matriciel diélectrique dans lequel sont intégrées des particules électroconductrices à répartition aléatoire selon un degré de remplissage compris dans l'intervalle 0,03-0,15.
PCT/DE2011/001902 2010-10-29 2011-10-27 Revêtement composite métallique présentant une transmissivité optique élevée dans le spectre visible Ceased WO2012055397A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102010050110A DE102010050110B3 (de) 2010-10-29 2010-10-29 Metall-Komposit-Beschichtung mit hoher optischer Transmissivität im visuellen Spektrum
DE102010050110.7 2010-10-29

Publications (1)

Publication Number Publication Date
WO2012055397A1 true WO2012055397A1 (fr) 2012-05-03

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PCT/DE2011/001902 Ceased WO2012055397A1 (fr) 2010-10-29 2011-10-27 Revêtement composite métallique présentant une transmissivité optique élevée dans le spectre visible

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DE (1) DE102010050110B3 (fr)
WO (1) WO2012055397A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112059168A (zh) * 2020-08-08 2020-12-11 福达合金材料股份有限公司 基于纳米银线改性和3d梯度打印制备银金属氧化物电接触材料的方法及其产品

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102011113571B4 (de) 2011-09-19 2013-08-01 Christian-Albrechts-Universität Zu Kiel Absorberschicht für den VIS- und/oder NIR-Spektralbereich

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WO2004092439A2 (fr) * 2003-04-10 2004-10-28 Christian-Albrechts-Univer Sität Zu Kiel Procede de fabrication de nanocomposites metal-polymere
US20050088078A1 (en) 2003-01-28 2005-04-28 Mei-Rurng Tseng Organic electroluminescent device
US20050201717A1 (en) * 2004-03-11 2005-09-15 Sony Corporation Surface plasmon resonance device
JP2007035430A (ja) * 2005-07-27 2007-02-08 Seiko Instruments Inc 有機発光素子
US20070069199A1 (en) * 2005-09-26 2007-03-29 Osram Opto Semiconductors Gmbh Interface conditioning to improve efficiency and lifetime of organic electroluminescence devices
US20070114523A1 (en) * 2005-11-18 2007-05-24 Manabu Oumi Electroluminescence element and display device using the same
WO2008111949A2 (fr) * 2006-07-05 2008-09-18 Optimax Technology Corporation Nanotechnologie de métal pour des applications d'affichage et optiques avancées
DE102007061979A1 (de) 2007-12-21 2009-06-25 Giesecke & Devrient Gmbh Sicherheitselement
EP2109147A1 (fr) 2008-04-08 2009-10-14 FOM Institute for Atomic and Molueculair Physics Cellule photovoltaïque avec nano-structures à génération de résonance à plasmons de surface
WO2009141903A1 (fr) * 2008-05-21 2009-11-26 パイオニア株式会社 Elément électroluminescent organique
EP2139045A1 (fr) 2008-04-09 2009-12-30 OOO "Novye Energeticheskie Tehnologii" Convertisseur de rayonnement electromagnetique

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US20050088078A1 (en) 2003-01-28 2005-04-28 Mei-Rurng Tseng Organic electroluminescent device
WO2004092439A2 (fr) * 2003-04-10 2004-10-28 Christian-Albrechts-Univer Sität Zu Kiel Procede de fabrication de nanocomposites metal-polymere
DE10316379B4 (de) 2003-04-10 2006-06-01 Christian-Albrechts-Universität Zu Kiel Verfahren zur Herstellung von Metall-Polymer-Nanokompositen
US20050201717A1 (en) * 2004-03-11 2005-09-15 Sony Corporation Surface plasmon resonance device
JP2007035430A (ja) * 2005-07-27 2007-02-08 Seiko Instruments Inc 有機発光素子
US20070069199A1 (en) * 2005-09-26 2007-03-29 Osram Opto Semiconductors Gmbh Interface conditioning to improve efficiency and lifetime of organic electroluminescence devices
US20070114523A1 (en) * 2005-11-18 2007-05-24 Manabu Oumi Electroluminescence element and display device using the same
WO2008111949A2 (fr) * 2006-07-05 2008-09-18 Optimax Technology Corporation Nanotechnologie de métal pour des applications d'affichage et optiques avancées
DE102007061979A1 (de) 2007-12-21 2009-06-25 Giesecke & Devrient Gmbh Sicherheitselement
EP2109147A1 (fr) 2008-04-08 2009-10-14 FOM Institute for Atomic and Molueculair Physics Cellule photovoltaïque avec nano-structures à génération de résonance à plasmons de surface
EP2139045A1 (fr) 2008-04-09 2009-12-30 OOO "Novye Energeticheskie Tehnologii" Convertisseur de rayonnement electromagnetique
WO2009141903A1 (fr) * 2008-05-21 2009-11-26 パイオニア株式会社 Elément électroluminescent organique
EP2287939A1 (fr) 2008-05-21 2011-02-23 Pioneer Corporation Elément électroluminescent organique

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Title
CESARIO ET AL.: "Coupling localized and extended plasmons to improve the light extraction through metal films", OPTICS EXPRESS, vol. 15, no. 17, 2007, pages 10533 - 10539, XP055021338, DOI: doi:10.1364/OE.15.010533
JEAN CESARIO ET AL: "Coupling localized and extended plasmons to improve the light extraction through metal films", OPTICS EXPRESS, vol. 15, no. 17, 1 January 2007 (2007-01-01), pages 10533, XP055021338, ISSN: 1094-4087, DOI: 10.1364/OE.15.010533 *
KILDISHEV ET AL.: "Negative refractive index in optics of metal-dielectric composites", J. OPT. SOC. AM. B, vol. 23, no. 3, 2006, pages 423 - 433

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112059168A (zh) * 2020-08-08 2020-12-11 福达合金材料股份有限公司 基于纳米银线改性和3d梯度打印制备银金属氧化物电接触材料的方法及其产品

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