DE102007018540A1 - Electrically conductive composition for use as transparent or non-transparent conductive coating for resistance heating elements e.g. for heating disks, comprises electrically conductive polymer, carbon nanotubes and baytron - Google Patents

Electrically conductive composition for use as transparent or non-transparent conductive coating for resistance heating elements e.g. for heating disks, comprises electrically conductive polymer, carbon nanotubes and baytron Download PDF

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DE102007018540A1
DE102007018540A1 DE102007018540A DE102007018540A DE102007018540A1 DE 102007018540 A1 DE102007018540 A1 DE 102007018540A1 DE 102007018540 A DE102007018540 A DE 102007018540A DE 102007018540 A DE102007018540 A DE 102007018540A DE 102007018540 A1 DE102007018540 A1 DE 102007018540A1
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electrically conductive
transparent
carbon nanotubes
conductive polymer
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Harun Erismis
Mohammed Hamidul Haque
Daniel Georg Weis
Klaus Dr.rer.nat. Hying
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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    • 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
    • H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D165/00—Coating compositions based on macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Coating compositions based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D165/00—Coating compositions based on macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Coating compositions based on derivatives of such polymers
    • C09D165/02—Polyphenylenes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/24—Electrically-conducting paints
    • 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
    • H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
    • H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
    • H01B1/124—Intrinsically conductive polymers
    • H01B1/127—Intrinsically conductive polymers comprising five-membered aromatic rings in the main chain, e.g. polypyrroles, polythiophenes
    • 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
    • H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
    • H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
    • H01B1/124—Intrinsically conductive polymers
    • H01B1/128—Intrinsically conductive polymers comprising six-membered aromatic rings in the main chain, e.g. polyanilines, polyphenylenes
    • 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
    • H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
    • H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
    • H05B3/146—Conductive polymers, e.g. polyethylene, thermoplastics
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
    • C08G2261/10—Definition of the polymer structure
    • C08G2261/14—Side-groups
    • C08G2261/142—Side-chains containing oxygen
    • C08G2261/1424—Side-chains containing oxygen containing ether groups, including alkoxy
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
    • C08G2261/30—Monomer units or repeat units incorporating structural elements in the main chain
    • C08G2261/31—Monomer units or repeat units incorporating structural elements in the main chain incorporating aromatic structural elements in the main chain
    • C08G2261/312—Non-condensed aromatic systems, e.g. benzene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
    • C08G2261/30—Monomer units or repeat units incorporating structural elements in the main chain
    • C08G2261/32—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain
    • C08G2261/322—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain non-condensed
    • C08G2261/3223—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain non-condensed containing one or more sulfur atoms as the only heteroatom, e.g. thiophene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
    • C08G2261/50—Physical properties
    • C08G2261/51—Charge transport
    • C08G2261/512—Hole transport
    • C—CHEMISTRY; METALLURGY
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    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
    • C08G2261/70—Post-treatment
    • C08G2261/79—Post-treatment doping
    • C08G2261/794—Post-treatment doping with polymeric dopants
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/041—Carbon nanotubes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L65/00—Compositions of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Compositions of derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L65/00—Compositions of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Compositions of derivatives of such polymers
    • C08L65/02—Polyphenylenes
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2214/00—Aspects relating to resistive heating, induction heating and heating using microwaves, covered by groups H05B3/00, H05B6/00
    • H05B2214/04—Heating means manufactured by using nanotechnology

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  • Spectroscopy & Molecular Physics (AREA)
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  • Paints Or Removers (AREA)
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Abstract

The electrically conductive composition comprises an electrically conductive polymer, carbon nanotubes and baytron. The electrically conductive polymer is selected from poly(3,4-ethylenedioxythiophene), polythiophene, polypyrrole, polyaniline, polyacethylene, polydiphenylamine, poly para-phenylene, poly para-phenylene vinylene, poly para phenylene sulfide or their derivatives, preferably from poly(3,4-ethylenedioxythiophene). The electrically conductive polymer is present as polymer radical cation. The polymer radical cation responds to a coordination bond with a polyanion. An independent claim is also included for a method for producing the electrically conductive composition, which involves dispersing carbon nanotubes in a conductive polymer.

Description

Heutzutage werden in vielen Bereichen heizbare Oberflächen benötigt. Dies geschieht teilweise durch die Verwendung von Metalldrähten, die zu einer elektrischen Widerstandsheizung miteinander verbunden werden oder durch Aufspritzen von Kupfer auf ein geeignetes Substrat, um eine elektrische Widerstandsheizung aufzubauen. Das Aufspritzen von Kupfer auf die Rückseite von Badezimmerspiegeln ist ein Anwendungsbeispiel für eine solche flächige elektrische Widerstandsheizung. Nachteilig an diesen elektrischen Widerstandsheizungen ist, dass sie erstens nicht optisch transparent und damit nicht anwendbar sind, wenn Transparenz erforderlich ist. Außerdem sind solche elektrischen Widerstandsheizungen sehr aufwändig und teuer in der Herstellung. Schließlich sind sie bei Beschädigungen nur schwer wieder in Stand zu setzen.nowadays In many areas, heatable surfaces are needed. This happens partially through the use of metal wires leading to an electrical Resistance heating are connected to each other or by spraying of copper on a suitable substrate to build an electrical resistance heater. Spraying copper onto the back of bathroom mirrors is an application example for such a plane electrical resistance heating. A disadvantage of these electrical resistance heaters is that, firstly, they are not optically transparent and therefore not applicable when transparency is required. Besides, they are Such electrical resistance heaters very expensive and expensive in the production. After all, they are damaged difficult to repair.

Alternativ ist es möglich, elektrische Widerstandsheizungen mit Hilfe von elektrisch leitfähigen Polymeren herzustellen. Diese elektrisch leitfähigen Polymere sind jedoch thermisch nicht besonders stabil. Dies ist naturgemäß bei einer elektrischen Widerstandsheizung ein besonders großer Nachteil.alternative Is it possible, electrical resistance heaters with the aid of electrically conductive polymers manufacture. However, these electrically conductive polymers are thermally not very stable. This is naturally one electrical resistance heating a particularly big disadvantage.

Allerdings sind am Markt elektrisch leitfähige Polymere erhältlich, die den Vorteil aufweisen, dass sie transparent sind. Ein Beispiel für solche Polymere ist PEDOT, das auch unter dem Handelsnamen Baytron von der Bayer AG vertrieben wird.Indeed are electrically conductive in the market Polymers available, which have the advantage that they are transparent. An example for such Polymers is PEDOT, which is also available under the trade name Baytron from the Bayer AG is distributed.

Der Erfindung liegt die Aufgabe zugrunde, eine elektrisch 4 leitfähige und bei Bedarf auch transparente Zusammensetzung bereitzustellen, die erstens eine ausreichende thermische Stabilität aufweist, deren Transparenz ausreichend hoch ist und die noch dazu kostengünstig in der Herstellung und einfach in der Verarbeitung ist.Of the Invention is the object of an electrically conductive 4 and if necessary, also to provide transparent composition which first, has sufficient thermal stability, their transparency is sufficiently high and the moreover inexpensive in the production and is easy to work with.

Diese Aufgabe wird erfindungsgemäß dadurch gelöst, dass die elektrisch leitfähige Zusammensetzung mindestens ein leitfähiges Polymer und Carbon-Nanotubes (CNT) enthält.These Task is inventively characterized solved, that the electrically conductive Composition of at least one conductive polymer and carbon nanotube Contains (CNT).

Es hat sich überraschenderweise bei praktischen Versuchen herausgestellt, dass durch das Dispergieren von Carbon-Nanotubes in sehr geringen Mengen in ein elektrisch leitendes Polymer oder eine Mischung elektrisch leitender Polymere erstens die Leitfähigkeit der elektrisch leitenden Polymere verbessert werden kann, ohne die Transparenz derselben nennenswert zu beeinträchtigen. Zweitens hat es sich herausgestellt, dass die thermische Stabilität der elektrisch leitenden Polymere durch die Zugabe der Carbon-Nanotubes deutlich erhöht wird. Damit wird der Einsatz von elektrisch leitenden Polymere als elektrische Widerstandsheizung in vielen Anwendungsgebieten überhaupt erst ermöglicht.It has surprisingly in practical experiments proved that by dispersing of carbon nanotubes in very small quantities in an electrically conductive polymer or a mixture of electrically conductive polymers, first, the conductivity the electrically conductive polymer can be improved without the Significantly affect their transparency. Second, it has proved that the thermal stability of the electrically conductive Polymer is significantly increased by the addition of carbon nanotubes. Thus, the use of electrically conductive polymers as electrical Resistance heating in many application areas made possible.

Es ist somit möglich, transparente elektrische Widerstandsheizungen bestehend aus elektrisch leitfähigen Polymeren und Carbon-Nanotubes bereitzustellen, wobei sich eine Transparenz von 95% ohne Weiteres realisieren lässt.It is thus possible transparent electrical resistance heaters consisting of electrical conductive To provide polymers and carbon nanotubes, wherein a Transparency of 95% can be realized easily.

Eine besonders vorteilhafte Ausgestaltung der erfindungsgemäßen Zusammensetzung ist dadurch gekennzeichnet, dass sie einen Komplex eines elektrisch leitfähigen Polymers mit einem Polyanion enthält. Weiter Beispiele für elektrisch leitfähige Polymere sind: Polypyrrole, Polyanilin, Polythiophene, Polyparaphenylene, Polyparaphenylen-Vinylene und deren Derivate.A particularly advantageous embodiment of the composition according to the invention is characterized in that it is a complex of an electric conductive Contains polymer with a polyanion. Further examples of electrical conductive Polymers are: polypyrroles, polyaniline, polythiophenes, polyparaphenylenes, Polyparaphenylene-vinylenes and their derivatives.

Carbon-Nanotubes sind ein hinlänglich bekanntes und im Handel verfügbares Material. Sie werden beispielsweise von der Firma Bayer Material Science unter dem Handelsnamen Baytubes oder von Carbon Nanotechnologie Inc. unter dem Handelsnamen CNI Buckytube vertrieben.Carbon nanotubes are a sufficient known and commercially available Material. They are for example from the company Bayer Material Science under the trade name Baytubes or carbon nanotechnology Inc. under the trade name CNI Buckytube.

In praktischen Versuchen hat es sich als ausreichend erwiesen, 0,01 Gew.-% Carbon-Nanotubes in mindestens einen elektrisch leitfähigen Polymer einzudispergieren, um erstens die gewünschte elektrische Verbesserung der elektrischen Leitfähigkeit und zweitens die hohe Transparenz des Polymers weitestgehend zu erhalten. Selbstverständlich kann durch die Zugabe von größeren Mengen von Carbon-Nanotubes die elektrische Leitfähigkeit noch weiter verbessert werden, wobei dies zu einer Verringerung der Transparenz führt. Allerdings ist, wie beispielsweise bei getönten Autoscheiben, es oftmals gewünscht, dass die Transparenz auf einen Wert von beispielsweise 70% reduziert wird. Eine solche vorgegebene Transparenz ist ohne Weiteres durch die Zugabe der Anteile an Carbon-Nanotubes sehr genau einstellbar.In Practical tests have proved satisfactory, 0.01 Wt .-% carbon nanotubes in at least one electrically conductive polymer to firstly, to the desired electrical improvement the electrical conductivity and second, the high transparency of the polymer as much as possible receive. Of course can by the addition of larger quantities Carbon Nanotubes further improves electrical conductivity which leads to a reduction in transparency. Indeed is, for example, when toned Car windows, it is often desired that reduces the transparency to a value of, for example, 70% becomes. Such a given transparency is easily through the addition of the proportions of carbon nanotubes can be set very precisely.

Es hat sich bei praktischen Versuchen ebenfalls als ausreichend erwiesen, wenn 0,5 Gewichts-% Carbon-Nanotubes in das oder die. Polymere dispergiert werden. Allerdings ist es bei Bedarf auch möglich, mehr als 0,5 Gewichts-% einzudispergieren.It has also proved to be sufficient in practical experiments, if 0.5% by weight of carbon nanotubes in the or. Dispersed polymers become. However, it is also possible if needed, more than 0.5% by weight making sure there.

Durch die erfindungsgemäß beanspruchte Zusammensetzung eröffnen sich eine Vielzahl von neuen Anwendungsgebieten elektrischer Widerstandsheizungen, die auf verschiedensten Oberflächen aufgebracht werden können. Es ist beispielsweise möglich, mit geringen Zugaben von Carbon-Nanotubes elektrische Widerstandselemente mit hoher Transparenz (> 95%) bereitzustellen, die so temperaturstabil sind, dass sie auch als Heizelement einsetzbar sind. Durch die Zugabe größerer Mengen von Carbon-Nanotubes kann die elektrische Leitfähigkeit noch weiter verbessert werden, so dass Beschichtungen aus dieser Zusammensetzung auch als Heizlack eingesetzt werden können.By claimed in the invention Open composition a multitude of new fields of application of electrical resistance heaters, on different surfaces can be applied. For example, it is possible with low additions of carbon nanotubes electrical resistance elements with high transparency (> 95%) To provide that are so stable in temperature that they also as Heating element can be used. By adding larger amounts of carbon nanotubes can the electrical conductivity to be further improved, making coatings from this Composition can also be used as Heizlack.

Ein Anwendungsbeispiel für einen solchen Heizlack ist die Beheizung eines Autospiegels. Dazu wird der Heizlack auf der Rückseite des Autospiegels aufgetragen. Dieser Heizlack muss, wenn er auf der Rückseite eines Spiegels angebracht wird, naturgemäß nicht transparent sein. In diesem Fall dient das Polymer als Matrix für die Carbon-Nanotubes. Dadurch erreichen die Polymere, auch wenn sie nicht transparent sind, die erforderliche thermische Stabilität.One Application example for such a Heizlack is the heating of a car mirror. To is the Heizlack on the back applied to the car mirror. This heating varnish must when he is on the back a mirror is mounted, by nature not be transparent. In In this case, the polymer serves as a matrix for the carbon nanotubes. Thereby The polymers, even if they are not transparent, achieve the required thermal stability.

Als besonders vorteilhaft hat es sich erwiesen, wenn die Carbon-Nanotubes mittels eines Dreiwalzwerk in das oder die elektrisch leitfähigen Polymere dispergiert werden. Bei praktischen Versuchen hat es sich als vorteilhaft herausgestellt, wenn in dem Dreiwalzwerk ein Spalt von 5 μm Dicke eingestellt wird. Dann nämlich sind die Scherkräfte des Dreiwalzwerks so groß, dass die Carbon-Nanotubes deagglomeriert werden, also fein und gleichmäßig verteilt in dem Polymer vorliegen.When It has proven particularly advantageous if the carbon nanotubes by means of a three-roll mill in the one or more electrically conductive polymers be dispersed. In practical experiments, it has proved to be advantageous pointed out when set in the three-roll mill, a gap of 5 microns thickness becomes. Then that is are the shear forces of the three-roll mill so big that the carbon nanotubes are deagglomerated, so finely and evenly distributed present in the polymer.

Alternativ ist es auch möglich, die Carbon-Nanotubes zum Beispiel durch Ultraschall in den Polymeren zu dispergieren.alternative it is also possible the carbon nanotubes for example by ultrasound in the polymers too disperse.

Um das erfindungsgemäße leitfähige Komposit herstellen zu können, sind verschiedene Schritte nötig. Da das leitfähige Polymer für den Einsatz im Dreiwalzwerk zu dünnflüssig ist, muss dessen Viskosität zuvor erhöht werden. Nur dann ist es möglich mittels dieses Verfahrens die CNTs effektiv darin zu dispergieren.Around the conductive composite according to the invention to be able to produce Different steps are necessary. There the conductive one Polymer for the use in three-roll mill is too fluid, must its viscosity previously increased become. Only then is it possible using this method to effectively disperse the CNTs therein.

Dazu werden dem PEDOT die Lösungsmittel ausgedampft. Es hat sich gezeigt, dass sich eine gute Viskosität bei der Hälfte des ursprünglichen Volumens einstellt. In diesem Zustand kann es nun mit den CNTs vermischt und einem Dreiwalzwerk zugeführt werden. Die Prozessdauer ist je nach CNT-Gehalt verschieden und beträgt für geringe CNT-Anteile (z. B. 0,01 wt%) 30 Minuten, kann aber mehr als 120 Minuten für höhere CNT-Anteile in Anspruch nehmen (z. B. 0,5 wt%).To become the solvent for the PEDOT evaporated. It has been shown that a good viscosity in the half of the original one Volume. In this state, it can now be mixed with the CNTs and fed to a three-roll mill become. The duration of the process differs depending on the CNT content and is for low CNT contents (eg, 0.01 wt%) for 30 minutes, but may exceed 120 Minutes for higher CNT shares claim (eg 0.5 wt%).

Das Dreiwalzwerk wird dabei in verschiedenen Modi betrieben. Anfangs wird ein größerer Spalt (50 μm) eingestellt, um größere Agglomerate aufzuspalten. Die Drehzahl beträgt dabei zum Beispiel 180 min–1 für die vorderste Walze und nimmt um je ein drittel zu den nächsten zwei Walzen ab. Dadurch herrscht zwischen den Walzen, wo die eigentliche Dispergierung stattfindet, eine Relativbewegung.The three-roll mill is operated in different modes. Initially, a larger gap (50 microns) is set to split larger agglomerates. The speed is, for example, 180 min -1 for the foremost roller and decreases by one third each to the next two rollers. As a result, there is a relative movement between the rollers where the actual dispersion takes place.

Je nach Qualität der Dispersion (optische Prüfung zwischen zwei Objektträgern) wird die Spaltbreite schrittweise verkleinert bis auf 5 μm.ever after quality the dispersion (optical test between two slides) The gap width is gradually reduced down to 5 μm.

Bei der Eindispergierung der CNTs mittels Ultraschall, muss das leitfähige Polymer nicht weiter verdünnt werden. Hier können die CNTs mittels der üblichen Einstellungen des Ultraschallgerätes (36W–60W; 40%–60% Amplitude; Dauer 10–60 Minuten) direkt in das leitfähige Polymer eingearbeitet werden. Insbesondere kommen hier funktionalisierte CNTs zum Einsatz, die sich in Wasser dispergieren lassen (PEDOT besteht zum größten Teil aus Wasser).at By dispersing the CNTs by means of ultrasound, the conductive polymer must not diluted further become. here we can the CNTs by the usual Settings of the ultrasound device (36W-60W, 40% -60% amplitude; Duration 10-60 Minutes) directly into the conductive Polymer are incorporated. In particular, functionalized ones come here CNTs are used which can be dispersed in water (PEDOT exists for the most part of water).

Es ist möglich, die auf diese Weise gewonnene elektrisch leitfähige Zusammensetzung beispielsweise durch Spritzen, Sprühen, Rakeln, Spin-Coating (Rotationsbeschichtung), Dip-Coating (Tauchbeschichtung), Streichen mit einem Pinsel oder Sprühen auf das Substrat aufzubringen.It is possible, the electrically conductive composition obtained in this way, for example Spraying, spraying, Squeegee, spin-coating, dip-coating, brushing with a brush or spray to apply to the substrate.

Anschließend wird das Lösungsmittel, welches häufig aus Wasser besteht, durch Erwärmen aus der Zusammensetzung ausgetrieben und dadurch die erfindungsgemäße elektrisch leitfähige Zusammensetzung ausgehärtet. Anschließend ist es in der Regel noch erforderlich, die erfindungsgemäße Zusammensetzung elektrisch zu kontaktieren.Subsequently, will the solvent, which often consists of water, by heating expelled from the composition and thereby the invention electrically conductive Hardened composition. Subsequently As a rule, it is still necessary for the composition according to the invention to be electrically to contact.

Beispiele erfindungsgemäßer elektrisch leitfähiger und transparenter Zusammensetzungen sind in der nachfolgenden Tabelle zusammengestellt: Komposit 1 Komposit 2 Komposit 3 Komposit 4 Leitfähiges Polymer (CP) [Gew.-%] 1,1 1,1 1,1 1,1 Carbon-Nanotubes (CNT) [Gew.-%] 0,01 0,02 0,04 0,05 Drehzahl Dreiwalzwerk [1/min] 180–600 180–600 180–600 180–600 Oberflächen-widerstand [Ω/Sq] 80 80 80 80 Transparenz [%] 70 76 66 64 Examples of inventive electrically conductive and transparent compositions are listed in the following table: Composite 1 Composite 2 Composite 3 Composite 4 Conductive polymer (CP) [% by weight] 1.1 1.1 1.1 1.1 Carbon nanotubes (CNT) [% by weight] 0.01 0.02 0.04 0.05 Speed three-roll mill [1 / min] 180-600 180-600 180-600 180-600 Surface resistance [Ω / sq] 80 80 80 80 Transparency [%] 70 76 66 64

Mögliche Anwendungen der erfindungsgemäßen elektrisch leitfähigen Zusammensetzung sind Fußbodenheizungen, Handtuchtrockner, die Heizung von Spiegeln oder Glasscheiben, Sitzheizungen und Heizung von Griffen, beispielsweise an dem Lenker eines Motorrads, und überall dort, wo transparente und/oder nicht transparente Oberflächen beheizt werden sollen.Possible applications the invention electrically conductive Composition are underfloor heating, towel dryer, the heating of mirrors or glass panes, seat heaters and heating of handles, for example on the handlebars of a motorcycle, and everywhere, where transparent and / or non-transparent surfaces are heated should be.

Alle in den Ausführungsbeispielen und den Patentansprüchen beschriebenen Merkmale können sowohl einzeln als auch in beliebiger Kombination miteinander erfindungswesentlich sein.All in the embodiments and the claims described features both individually and in any combination with each other invention essential be.

Claims (22)

Elektrisch leitfähige Zusammensetzung enthaltend mindestens ein elektrisch leitfähiges Polymer (CP) und Carbon-Nanotubes.Containing electrically conductive composition at least one electrically conductive Polymer (CP) and carbon nanotubes. Zusammensetzung nach Anspruch 1, dadurch gekennzeichnet, dass das elektrisch leitfähige Polymere ausgewählt ist aus elektrisch leitfähigen Polymeren aus Poly(3,4-ethylendioxythiophen), Polythiophen, Polypyrrol, Polyanilin, Polyacethylen, Polydiphenylamin, Polyparaphenylen, Polyparaphenylenvinylen, Polyparphenylensulfid und deren Derivate.Composition according to Claim 1, characterized that the electrically conductive Polymers selected is made of electrically conductive Polymers of poly (3,4-ethylenedioxythiophene), Polythiophene, polypyrrole, polyaniline, polyacetylene, polydiphenylamine, Polyparaphenylen, Polyparaphenylenvinylen, Polyparphenylensulfid and their derivatives. Zusammensetzung nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass das elektrisch leitfähige Polymer als polymeres Radikalkation vorliegt.Composition according to Claim 1 or 2, characterized that the electrically conductive Polymer is present as a polymeric radical cation. Zusammensetzung nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass das polymere Radikalkation eine koordinative Bindung mit einem Polyanion eingeht.Composition according to Claim 1 or 2, characterized that the polymeric radical cation has a coordinative bond with a Polyanion arrives. Zusammensetzung nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass es sich bei dem elektrisch leitfähigen Polymer um elektrisch leitfähiges Poly(3,4-ethylendioxythiophen) (PEDOT) handelt.Composition according to Claim 1 or 2, characterized that the electrically conductive polymer is electrical conductive Poly (3,4-ethylenedioxythiophene) (PEDOT) acts. Zusammensetzung nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass es sich bei dem Polyanion um Polystyrrolsulfonat handelt.Composition according to Claim 1 or 2, characterized that the polyanion is polystyrrolesulfonate. Zusammensetzung nach einem der vorhergehenden Ansprüche dadurch gekennzeichnet, dass sie „Baytron" enthält.A composition according to any one of the preceding claims characterized in that it contains "Baytron". Zusammensetzung nach einem der vorhergehenden Ansprüche dadurch gekennzeichnet, dass es sich bei den Carbon-Nanotubes (CNT) um einwandige (single-wall), zweiwandige (double-wall), mehrwandige (multi-wall) und/oder gebündelte (bundled) Carbon-Nanotubes oder einer Mischung aus zwei oder mehrer dieser Carbon-Nanotube-Arten handelt.A composition according to any one of the preceding claims characterized in that the carbon nanotubes (CNT) are single-walled, double-walled, multi-walled and / or bundled Carbon nanotubes or a mixture of two or more of these Carbon nanotube species acts. Zusammensetzung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass der Anteil an Carbon-Nanotubes (CNT) in der Dispersion mindestens 0,01 Gewichts-Prozente (0,01 Gew.-%) und maximal 25 Gewichts-Prozente (25 Gew.-%) enthält.Composition according to one of the preceding claims, characterized characterized in that the proportion of carbon nanotubes (CNT) in the dispersion at least 0.01% by weight (0.01% by weight) and at most 25% by weight (25% by weight) contains. Zusammensetzung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass sie im Vergleich zu den Ausgangskomponenten bei gleicher Leitfähigkeit eine höhere Transparenz aufweist.Composition according to one of the preceding claims, characterized characterized in that they compared to the starting components with the same conductivity a higher one Has transparency. Zusammensetzung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass sie im Vergleich zu den Ausgangskomponenten bei gleicher Transparenz ein höhere Leitfähigkeit aufweist. Ausgangskomponenten bei gleicher Transparenz ein höhere Leitfähigkeit aufweist.Composition according to any one of the preceding claims, characterized in that it is in the Compared to the starting components with the same transparency has a higher conductivity. Output components with the same transparency has a higher conductivity. Zusammensetzung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass sie im Vergleich zu einer Schicht aus leitfähigen Polymeren eine höhere thermische Stabilität aufweist.Composition according to one of the preceding claims, characterized characterized in that they are compared to a layer of conductive polymers a higher one thermal stability having. Verfahren zur Herstellung einer elektrisch leitfähigen Zusammensetzung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Carbon-Nanotubes (CNT) in mindestens. einem leitfähigen Polymer (CP) dispergiert werden.Process for the preparation of an electrically conductive composition according to one of the preceding claims, characterized that the carbon nanotubes (CNT) in at least. a conductive polymer (CP) are dispersed. Verfahren nach Anspruch 13, dadurch gekennzeichnet, dass die Carbon-Nanotubes (CNT) in mindestens einem leitfähigen Polymer (CP) mit dem Dreiwalzwerk dispergiert werden.Method according to claim 13, characterized in that that the carbon nanotubes (CNT) in at least one conductive polymer (CP) are dispersed with the three-roll mill. Verfahren nach Anspruch 13, dadurch gekennzeichnet, dass die Carbon-Nanotubes (CNT) in mindestens einem leitfähigen Polymer (CP) mit Ultraschall dispergiert werden.Method according to claim 13, characterized in that that the carbon nanotubes (CNT) in at least one conductive polymer (CP) are dispersed with ultrasound. Verfahren nach einem der Ansprüche 13 bis 15, dadurch gekennzeichnet, dass die Viskosität von mindestens einem leitfähigen Polymer (CP) durch Zugabe einer Flüssigkeit, insbesondere von Wasser, vor dem Dispergieren der Carbon-Nanotubes herabgesetzt wird.Method according to one of claims 13 to 15, characterized that the viscosity of at least one conductive Polymer (CP) by adding a liquid, in particular of Water is reduced before dispersing the carbon nanotubes. Verfahren nach einem der Ansprüche 13 bis 16, dadurch gekennzeichnet, dass das Auftragen der Dispersion auf ein Substrat durch ein Beschichtungsverfahren wie Rakeln, Aufstreichen, Aufsprühen, Drucken, Spin-Coating (Rotationsbeschichtung) und/oder Dip-Coating (Tauchen) erfolgt.Method according to one of claims 13 to 16, characterized that the application of the dispersion to a substrate by a coating process like doctoring, painting, spraying, Printing, spin coating (spin coating) and / or dip coating (Diving) takes place. Verfahren nach einem der Ansprüche 13 bis 17, dadurch gekennzeichnet, dass die Beschichtung eine oder mehrere elektrische Kontaktierungen aufweist.Method according to one of claims 13 to 17, characterized that the coating one or more electrical contacts having. Anwendung einer Zusammensetzung nach einem der Ansprüche 1 bis 12, dadurch gekennzeichnet, dass sie als transparente und/oder nichttransparente leitfähige Beschichtung für Widerstandsheizelemente beispielsweise zur Beheizung von Scheiben und Fenstern und Spiegeln, von Textilen und Tauchanzügen, als Fußboden- und Treppenheizung, zur Beheizung von Bildschirmen und PDAs (Touchscreens), Verkehrsschildern (enteisen) oder als Heizschicht zur Verhinderung von Kondensatbildung z. B. bei Kühlschrankfenstern dient.Use of a composition according to any one of claims 1 to 12, characterized in that they are transparent and / or non-transparent conductive Coating for Resistance heating elements, for example for heating windows and windows and mirrors, textiles and diving suits, as flooring and stair heating, for heating screens and PDAs (touch screens), Road signs (de-icing) or as a heating layer to prevent of condensation z. B. is used in refrigerator windows. Anwendung einer Zusammensetzung nach einem der Ansprüche 1 bis 12, dadurch gekennzeichnet, dass sie als transparente und/oder nichttransparente elektrische Kontaktierung eingesetzt werden kann.Use of a composition according to any one of claims 1 to 12, characterized in that they are transparent and / or non-transparent electrical contact can be used. Anwendung einer Zusammensetzung nach einem der Ansprüche 1 bis 12, dadurch gekennzeichnet, dass sie als transparente und/oder nichttransparente Antistatikbeschichtung eingesetzt werden kann.Use of a composition according to any one of claims 1 to 12, characterized in that they are transparent and / or non-transparent Antistatic coating can be used. Anwendung einer Zusammensetzung nach einem der Ansprüche 1 bis 12, dadurch gekennzeichnet, dass sie als transparente und/oder nichttransparente Beschichtung zur elektromagnetischen Verträglichkeit eingesetzt werden kann.Use of a composition according to any one of claims 1 to 12, characterized in that they are transparent and / or non-transparent Coating be used for electromagnetic compatibility can.
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