WO2016050598A1 - Électrode de carbone et procédé et dispositif pour la production de cette dernière - Google Patents

Électrode de carbone et procédé et dispositif pour la production de cette dernière Download PDF

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Publication number
WO2016050598A1
WO2016050598A1 PCT/EP2015/071951 EP2015071951W WO2016050598A1 WO 2016050598 A1 WO2016050598 A1 WO 2016050598A1 EP 2015071951 W EP2015071951 W EP 2015071951W WO 2016050598 A1 WO2016050598 A1 WO 2016050598A1
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WO
WIPO (PCT)
Prior art keywords
carbon electrode
carbon
electrode
heated
electrodes
Prior art date
Application number
PCT/EP2015/071951
Other languages
German (de)
English (en)
Inventor
Thomas Turek
Ulrich Kunz
Maik Becker
Henning Becker
Niels Bredemeyer
Christoph ROOSEN
Gregor Damian POLCYN
Peter Toros
Original Assignee
Thyssenkrupp Ag
Thyssenkrupp Industrial Solutions Ag
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 Thyssenkrupp Ag, Thyssenkrupp Industrial Solutions Ag filed Critical Thyssenkrupp Ag
Publication of WO2016050598A1 publication Critical patent/WO2016050598A1/fr

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/96—Carbon-based electrodes
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/042—Electrodes formed of a single material
    • C25B11/043—Carbon, e.g. diamond or graphene
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
    • H01M8/184—Regeneration by electrochemical means
    • H01M8/188—Regeneration by electrochemical means by recharging of redox couples containing fluids; Redox flow type batteries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Definitions

  • the present invention relates to a method for producing a carbon electrode, in particular for a redox-flow battery, wherein the carbon electrode by means of
  • Carbon electrode Another object of the invention is a device for producing a carbon electrode, in particular for a redox flow battery, through which the carbon electrode is heated by means of electricity.
  • Redox flow batteries (flow batteries) have two filled with liquid electrolytes
  • Half cells separated by a membrane.
  • an electrode is arranged, at which a reduction or an oxidation takes place.
  • the electrodes of such redox flow batteries are formed as carbon electrodes. Since the carbon of these carbon electrodes is usually present as graphite, the carbon electrodes are also referred to as graphite electrodes.
  • the carbon electrodes are typically porous so that they have a large electrochemically active surface area. However, these often have inadequate electrochemical activity, in particular due to the hydrophobic properties of the graphite.
  • Carbon electrode can be improved.
  • the object of the present invention is to provide a process for the production of
  • the method should allow the production of carbon electrodes with high active surface and good electrochemical activity at low cost.
  • the object is achieved by a method for producing a carbon electrode, in particular for a redox flow battery, comprising the step (a):
  • Carbon electrode heated by the current flowing in the carbon electrode electric current takes place directly in the material of the carbon electrode, so that the heating proceeds much faster than is possible in processes in which the heating of the carbon electrode takes place by supplying the heat from the outside.
  • the production of the electrode can be carried out with less time.
  • Electrode material can be targeted. When switching off the current that cools
  • Electrode material from quickly, so that, for example, controlled by the oxidation and total oxidation of the material can be prevented.
  • the current conducted through the carbon electrode can be a direct current or a
  • carbon electrodes consist at least partially or entirely of carbon.
  • the carbon electrode is formed as a graphite electrode.
  • the electrodes may contain fibers or be constructed entirely of fibers, such as a felt, nonwoven, scrim or paper.
  • electrodes based on fibers which are coated with carbon, in particular graphite are materials such as Felt, nonwoven, scrim or paper called, which can be obtained by carbonization and subsequent graphitization of polyacrylonitrile.
  • An advantageous embodiment of the method provides that the carbon electrode is heated in an oxygen-containing atmosphere.
  • the surface of the carbon electrode can be oxidized. It may be possible to add oxygenated functional groups to the surface of the
  • Carbon electrode are applied, which increase the electrochemical activity of the carbon electrode.
  • an air atmosphere or an oxygen-rich atmosphere is used.
  • the carbon electrode may be heated in a gas atmosphere containing, instead of the oxygen or in addition to the oxygen, at least one other element to alternatively or additionally apply the other element to the surface of the
  • An alternative preferred embodiment provides that the carbon electrode is heated in air atmosphere at reduced pressure, for example ⁇ 300 mbar, preferably ⁇ 200 mbar, more preferably ⁇ 100 mbar, even more preferably ⁇ 50 mbar.
  • Contact elements is contacted, via which the current is introduced into the carbon electrode.
  • the contact elements are preferably connected to a power source. Due to the high electrical conductivity of copper, the contact elements are particularly preferably formed of copper.
  • the contact elements may be formed, for example, as clamping devices, in which the carbon electrode can be clamped.
  • the clamping of the carbon electrode between the contact elements is advantageous for the treatment of carbon electrodes, which are designed plate-shaped or strip-like.
  • the contact elements for contacting the carbon electrode can be brought into abutment with the carbon electrode, for example, by pressing the contact elements onto the carbon electrode.
  • the contact elements are designed as conveying elements, via which the carbon electrode is conveyed.
  • the contact elements can fulfill a dual function in that they both contact and promote the carbon electrode.
  • By formed as conveying elements contact elements it is possible to perform the treatment of the surface in a continuous process.
  • the carbon electrode may be heated by the electric current flowing between the conveying elements while being conveyed by the conveying elements.
  • Such conveying elements are used, which are rotationally movable.
  • the conveying elements may for example be designed as rollers which engage the carbon electrode. Particularly preferred is the
  • Abut carbon electrode so that the contact of the moving carbon electrode can be improved.
  • Carbon electrode is band-shaped, z. B. as a roll, tape or
  • a band-shaped carbon electrode can be contacted in a continuous treatment process by contact elements designed as conveying elements, so that a region of the electrodes arranged between the contact elements
  • the carbon electrode is heated to a temperature of at least 400 ° C, preferably at least 800 ° C, more preferably at least 1200 ° C, so that at least partial oxidation of the surface of the carbon electrode in an oxygen-containing atmosphere is made possible.
  • the high temperatures may cause the carbon electrodes to glow during the treatment.
  • the carbon electrode is heated for a duration in the range between 0 s and 180 s, preferably in the range between 5 s and 120 s, particularly preferably in the range between 10 s and 60 s.
  • the inventive method for the production of carbon electrodes thus represents a very simple, fast and inexpensive method, the wettability and thus also to increase the electrochemical activity of such electrodes.
  • this method is safe from a safety point of view, since toxicologically harmful hazardous substances can be dispensed with.
  • the inventive method leads to a change in the physical
  • Another object of the present invention is therefore also a
  • Carbon electrode obtainable by a method as described above.
  • the material of the carbon electrode is heated by the internally generated heat so far that it burns locally at least on the surface.
  • the surface of the carbon electrode produced by the method according to the invention is roughened in comparison with the carbon electrodes known from the prior art
  • the above-mentioned object is further achieved by a device for producing a carbon electrode, in particular for a redox flow battery, by means of which the carbon electrode can be heated, wherein an electrical current for heating the carbon electrode through the carbon electrode can be conducted with the aid of the device.
  • a device for producing a carbon electrode in particular for a redox flow battery, by means of which the carbon electrode can be heated, wherein an electrical current for heating the carbon electrode through the carbon electrode can be conducted with the aid of the device.
  • Another object of the invention is an energy storage device containing a carbon electrode described above.
  • the energy store is preferably a redox flow battery, in particular a vanadium redox flow battery.
  • the invention relates to a fuel cell, the one described above
  • the invention further relates to a device for water electrolysis, which contains a carbon electrode described above.
  • a device for water electrolysis which contains a carbon electrode described above.
  • the carbon electrode, the energy storage, the fuel cell and the device for water electrolysis the same result advantageous effects as they have already been described in connection with the method according to the invention.
  • the carbon electrode and / or the energy store may alternatively or additionally be used.
  • FIG. 1 shows a first embodiment of a device according to the invention for producing a carbon electrode in a schematic representation.
  • FIG. 2 shows a second embodiment of a device according to the invention for producing a carbon electrode in a schematic representation.
  • FIG. 3 shows cyclic voltammograms of a carbon electrode produced by the process according to the invention and of a corresponding carbon electrode which was not obtained by the process according to the invention.
  • FIG. 4 shows a photograph taken by means of scanning electron microscopy
  • FIGS. 5-7 show images of the carbon electrodes obtained by the method according to the invention by means of scanning electron microscopy.
  • Fig. 8 shows characteristics of redox-flow batteries with carbon electrodes produced by the method of the present invention as compared with non-appropriately heated carbon electrodes.
  • the carbon electrodes 3, 30, referred to below, are used in particular as electrodes in energy stores, such as redox flow batteries. Since chemical reactions take place at these carbon electrodes 3, 30, it is desirable for the carbon electrodes 3, 30 to be as large as possible
  • Carbon electrodes 3, 30 are therefore preferably porous, so that the respective electrolyte can flow through the carbon electrodes 3, 30.
  • Carbon electrodes 3, 30 are so far permeable to the electrolyte.
  • the carbon electrodes 3, 30 are formed of a three-dimensional porous carbon material, particularly a carbon nonwoven fabric, a carbon felt, a carbon laminate, or a carbon paper.
  • FIG. 1 schematically shows a first exemplary embodiment of a device 1 for carrying out the method according to the invention for treating the surface of a carbon electrode 3.
  • the carbon electrode 3 is strip-shaped and has a substantially rectangular base area of 3 cm x 4 cm. The thickness of the
  • Carbon electrode 3 is in the range of 0.2 mm to 0.4 mm.
  • the carbon electrode may, for example, be a gas diffusion electrode (GDL, series H2315, Freudenberg, Germany). These are graphite felts made by carbonization and subsequent graphitization of polyacrylonitrile fibers.
  • Carbon electrode 3 is heated in the device 1 by an electric current is passed through the carbon electrode 3. Due to the electrical resistance of the material of the carbon electrode 3, the carbon electrode 3 is heated directly when current flows.
  • the strip-like carbon electrode 3 is clamped between two contact elements 3 made of copper.
  • the contact elements 4 are designed in the manner of terminals which clamp the carbon electrode 3.
  • the contact elements 4 are connected via lines 5 to a power source 6.
  • the contact elements 4 and the carbon electrode 3 are arranged within a container 2, which is traversed by a gas.
  • the container For introducing the gas into the container 2, the container has an inlet 7. Further, an outlet 8 is provided on the container 2, through which the gas exits the container.
  • Embodiment is used as gas air, possibly at reduced pressure (1 mbar), so that the heating of the carbon electrode 3 is carried out in an oxygen-containing atmosphere.
  • the carbon electrode 3 When heated, the carbon electrode 3 is partially oxidized, thereby increasing the electrochemical activity when used in the energy storage, such as
  • the redox flow battery increases.
  • a current, in particular a direct current, of about 10 A in the carbon electrode 3 through the carbon electrode is passed for a period of about 20 s, so that in the carbon electrode for a short time a power density between 1 kW / m 2 and 500 kW / m 2 , preferably between 2 kW / m 2 and 300 kW / m 2 , more preferably between 4 kW / m 2 and 250 kW / m 2 is generated.
  • the carbon electrode 3 is heated to a temperature of at least 400 ° C, preferably at least 800 ° C, more preferably at least 1200 ° C.
  • Improved carbon electrode 3 and increases the surface and thereby the
  • the method can also be used to improve the electrochemical activity of carbon electrodes 3 provided with a hydrophobic coating.
  • Such hydrophobic coatings may be, for example, microporous layers consisting of mixtures of carbon particles with polymeric additives.
  • the hydrophobic polymers decompose at the high temperatures achieved by the heating, whereby the wettability of the carbon electrode 3 improves.
  • a second embodiment of a device 10 for carrying out the method according to the invention for producing a carbon electrode 30 is shown schematically.
  • the contact elements 40 are formed according to the second embodiment as electrically connected to the power source 6 rotatably movable rollers.
  • the contact elements act insofar as
  • the device 10 and the method according to the second embodiment are advantageous in such carbon electrodes 30, which are formed band-shaped, ie as rolled up strip material are present.
  • the surface of such belt-shaped carbon electrodes 30 can be treated with the device 10 in a continuous process.
  • the device 10 has two pairs of rollers with two rollers rotating in the opposite direction. The rollers of a pair of rollers abut against the carbon electrode 30 on two opposite sides. At least one of the two roles of a
  • FIG. 3 shows two cyclic voltammograms of an untreated and a carbon electrode 3, 30 treated by the method according to the invention, wherein the curve of the untreated carbon electrode 3, 30 with the reference symbol A and that of FIG
  • treated carbon electrode 3, 30 is designated by the reference B.
  • the cyclic voltammograms show the course of the current I over the voltage U of
  • Carbon electrode 3, 30, A which is due to higher electrochemical activity and an increased surface area of the treated carbon electrode 3, 30, B.
  • FIG. 4 shows a recording of the surface of a fiber of a carbon electrode, which has not been heated by current flow, by means of scanning electron microscopy and magnified 10000 times.
  • the surface of this carbon electrode has a smooth, fine fibrous surface.
  • Fig. 5 is a corresponding receptacle of a fiber surface one after the
  • Carbon electrode was treated at 15 A in an air atmosphere at normal pressure.
  • the surface of the fiber of this carbon electrode has crater-shaped recesses which due to the treatment.
  • the crater-shaped depressions increase the surface area of the carbon electrode.
  • Fig. 6 shows a photograph of a surface of a carbon electrode exposed to an electric current of 20 A in an air atmosphere at normal pressure.
  • the surface also has crater-shaped recesses.
  • the wells are smaller in diameter than the wells observed on the 15A treated carbon electrode.
  • Fig. 7 there is shown a surface of a fiber of a carbon electrode treated at a current of 29 A in an air atmosphere at normal pressure.
  • the surface of this carbon electrode has dimples of a reduced diameter compared to the surface shown in Figs. Overall, the surface is roughened by the treatment according to the invention.
  • Fiber diameter of a plurality of fibers determined and an average calculated.
  • the results of this study as a function of the heat introduced for heating are shown in Table 1.
  • Power density is. By reducing the diameter of the fibers occurs a loss of material, which manifests itself in a lower weight of the treated carbon electrodes. It also increases with decreasing
  • the droplet sinking time was determined experimentally, namely the time that elapses until an 8 ⁇ drop applied to the surface of the carbon electrode is completely immersed in the
  • Carbon electrode sunk The liquid used was demineralized water and various vanadium electrolytes. It was found that those treated by the process according to the invention at flows of 15 A and higher
  • Carbon electrodes have a droplet sinking time of at most 1 s, while the droplet sinking times are greater than 60 s for untreated electrodes.
  • Carbon electrodes are due to the increased hydrophilicity of the process.
  • FIG. 8 shows characteristic curves of redox flow batteries which have a construction described in more detail in DE 10 2012 017 306 A1.
  • the characteristics of redox flow batteries with untreated carbon electrodes are denoted by the reference symbol A, while the characteristics of redox flow batteries whose carbon electrodes have been treated by the method according to the invention are designated by the reference symbol B.
  • the treated area of the carbon electrodes is 11 cm x 11 cm.
  • the treatment of the carbon electrodes was carried out with a current of 30 A at a voltage of 30 V for a period of 15 s.
  • a power density of 74.4 kW / m 2 was provided.
  • the state of charge (SoC) of the redox flow battery was 90% when the characteristics were recorded.
  • the illustration shows that the redox flow battery with untreated carbon electrodes at 500 A
  • the carbon electrode 3, 30 is heated by an electric current through the
  • Carbon electrode 3, 30 is passed. As a result, the electrochemical activity of the surface of the carbon electrode 3, 30 is increased with little expenditure of time. In the method according to the invention can be dispensed with the use of toxicologically harmful hazardous substances. Since the carbon electrode 3, 30 is heated immediately and this after heating rapidly cools and there are no other heat transfer, the risk that people can come into contact with hot parts, greatly reduced.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Sustainable Development (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Sustainable Energy (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Inert Electrodes (AREA)

Abstract

La présente invention concerne un procédé de production d'une électrode de carbone (3, 30), en particulier pour une batterie à flux redox, l'électrode de carbone (3, 30) étant chauffée en étant traversée par un courant, une électrode de carbone pouvant être obtenue par ce procédé ainsi qu'une batterie à flux redox contenant une électrode de carbone de ce type. Un autre objet de l'invention est un dispositif (1, 10) permettant de produire une électrode de carbone (3, 30), en particulier pour une batterie à flux redox, par l'intermédiaire de laquelle l'électrode de carbone (3, 30) peut être chauffée au moyen d'un courant.
PCT/EP2015/071951 2014-10-02 2015-09-24 Électrode de carbone et procédé et dispositif pour la production de cette dernière WO2016050598A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102014114402.3A DE102014114402A1 (de) 2014-10-02 2014-10-02 Kohlenstoffelektrode sowie Verfahren und Vorrichtung zu ihrer Herstellung
DE102014114402.3 2014-10-02

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WO2016050598A1 true WO2016050598A1 (fr) 2016-04-07

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WO (1) WO2016050598A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170250417A1 (en) * 2014-09-15 2017-08-31 United Technologies Corporation Regeneration of flow battery electrode
CN116742018A (zh) * 2023-08-14 2023-09-12 保定市数果信息技术有限公司 一种液流电池的石墨毡电极改性处理装置及其实施方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB797944A (en) * 1953-12-04 1958-07-09 Ruhrchemie Ag Improvements in or relating to the production of carbon electrodes

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Publication number Priority date Publication date Assignee Title
DE2731760A1 (de) * 1977-07-14 1979-02-01 Kloeckner Humboldt Deutz Ag Verfahren und vorrichtung zur herstellung gebrannter kohleanoden, insbesondere zur verwendung fuer die aluminium- schmelzflusselektrolyse
DE4126175A1 (de) * 1991-08-07 1993-02-11 Montanstahl Ag Profilwalzwerk Verfahren und vorrichtung zum erwaermen von elektrisch leitfaehigem material
JPH05185129A (ja) * 1992-01-17 1993-07-27 Sumitomo Metal Ind Ltd 金属板の圧延装置
DE102006009567B3 (de) * 2006-02-28 2007-06-06 Daimlerchrysler Ag Verfahren zur Herstellung einer Elektrode
DE102012017306A1 (de) 2012-09-03 2014-03-06 Thyssenkrupp Uhde Gmbh Elektrochemische Zelle vom Durchflusstyp

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB797944A (en) * 1953-12-04 1958-07-09 Ruhrchemie Ag Improvements in or relating to the production of carbon electrodes

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170250417A1 (en) * 2014-09-15 2017-08-31 United Technologies Corporation Regeneration of flow battery electrode
US10680259B2 (en) * 2014-09-15 2020-06-09 Raytheon Technologies Corporation Regeneration of flow battery electrode
CN116742018A (zh) * 2023-08-14 2023-09-12 保定市数果信息技术有限公司 一种液流电池的石墨毡电极改性处理装置及其实施方法
CN116742018B (zh) * 2023-08-14 2024-04-09 保定市数果信息技术有限公司 一种液流电池的石墨毡电极改性处理装置及其实施方法

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