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Der Decal-Prozess Zur Herstellung Katalysatorbeschichteter Membranen Für PEM-Brennstoffzellen

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Der Decal-Prozess Zur Herstellung Katalysatorbeschichteter Membranen Für PEM-Brennstoffzellen Konstantin Frölich DER DECAL-PROZESS ZUR HERSTELLUNG KATALYSATORBESCHICHTETER MEMBRANEN M-Brennstoffzellen FÜR PEM-BRENNSTOFFZELLEN E SCHRIFTENREIHE DES INSTITUTS ecal-Prozess für P FÜR ANGEWANDTE MATERIALIEN BAND 47 D K. FRÖLICH 47 Konstantin Frölich Der Decal-Prozess zur Herstellung katalysatorbeschichteter Membranen für PEM-Brennstoffzellen Schriftenreihe des Instituts für Angewandte Materialien Band 47 Karlsruher Institut für Technologie (KIT) Institut für Angewandte Materialien (IAM) Eine Übersicht aller bisher in dieser Schriftenreihe erschienenen Bände finden Sie am Ende des Buches. Der Decal-Prozess zur Herstellung katalysatorbeschichteter Membranen für PEM-Brennstoffzellen von Konstantin Frölich Dissertation, Karlsruher Institut für Technologie (KIT) Fakultät für Maschinenbau Tag der mündlichen Prüfung: 09. Oktober 2014 Impressum Karlsruher Institut für Technologie (KIT) KIT Scientific Publishing Straße am Forum 2 D-76131 Karlsruhe KIT Scientific Publishing is a registered trademark of Karlsruhe Institute of Technology. Reprint using the book cover is not allowed. www.ksp.kit.edu This document – excluding the cover – is licensed under the Creative Commons Attribution-Share Alike 3.0 DE License (CC BY-SA 3.0 DE): http://creativecommons.org/licenses/by-sa/3.0/de/ The cover page is licensed under the Creative Commons Attribution-No Derivatives 3.0 DE License (CC BY-ND 3.0 DE): http://creativecommons.org/licenses/by-nd/3.0/de/ Print on Demand 2015 ISSN 2192-9963 ISBN 978-3-7315-0334-7 DOI 10.5445/KSP/1000045306 Der Decal-Prozess zur Herstellung katalysatorbeschichteter Membranen für PEM-Brennstoffzellen Zur Erlangung des akademischen Grades Doktor der Ingenieurwissenschaften der Fakultät für Maschinenbau Karlsruher Institut für Technologie (KIT) genehmigte Dissertation Dipl.-Wi.-Ing. Konstantin Frölich Tag der mündlichen Prüfung: 09.10.2014 Hauptreferent: Prof. Dr. rer.nat. Michael Hoffmann 1. Koreferent: Prof. Dr. rer.nat. Helmut Ehrenberg 2. Koreferent: Prof. Dr.-Ing. Christina Roth Institut für Angewandte Materialien (IAM) Karlsruher Institut für Technologie (KIT) Kaiserstraße 12 76131 Karlsruhe, Deutschland Kurzfassung Bis zu einem Durchbruch im Massenmarkt müssen Brennstoffzellen- antriebe noch erhebliche Herausforderungen hinsichtlich Infrastruk- tur, Technologie und Kosten meistern. Aus Prozesssicht können dazu insbesondere effizientere Herstellungsverfahren beitragen. Dies be- trifft gerade die Herstellung der katalysatorbeschichteten Membran als Herzstück von Polymerelektrolytmembran-Brennstoffzellen (PEMFC). Diese soll über kontinuierliche Verfahren wie den sogenannten „Decal-Prozess“ erfolgen. Dabei werden die Elektroden über einen Tintenprozess auf die namensgebende Decal-Folie beschichtet und durch Heißpressen auf die Polymerelektrolytmembran übertragen. Ziel dieser Arbeit ist daher eine umfassende Untersuchung dieses Herstellungsprozesses, wobei sowohl das Prozessfenster zum Transfer der Elektroden von Decal-Folie auf Membran, als auch die Auswirkung der Prozessparameter im Tinten- und Transferprozess auf Struktur und Funktion der Materialien wie auch die Reproduzierbarkeit des Prozesses betrachtet werden soll. Wesentlicher Bestandteil ist dabei die Auswahl, Implementation und Bewertung von Charakterisie- rungsmethoden. Zur Untersuchung des Transfers der Elektrode von Decal-Folie auf Membran werden die drei wesentlichen Subaspekte der Adhäsion von Elektrode und Membran, der Kohäsion der Elektrode und der Adhäsi- on von Elektrode und Decal-Folie getrennt auf den Einfluss der Pro- zessparameter Zeit, Temperatur und Druck untersucht. Erstes erfolgt per T-Peel-Test am Modellsystem Membran / Membran, zweites per Double Cantilever Beam-Test und letztes per Zugscher-Test. Anschlie- ßend erfolgt eine Validierung der Ergebnisse durch Übertragsversu- che. So können erstmals die zugrunde liegenden Mechanismen auf- gedeckt und der Übertrag vorhergesagt werden. i Kurzfassung Zur Untersuchung der Auswirkung der Prozessparameter auf Struktur und Funktion werden Membran, Katalysator und Elektrode mit ex-situ Methoden wie auch die fertigen katalysatorbeschichteten Membra- nen mit in-situ Methoden in speziellen Brennstoffzellentestständen charakterisiert. Zur Untersuchung der Membranen werden Raster- elektronen- und Lichtmikroskopie, Zug- und Weiterreißprüfungen, Helium-Pyknometrie, Dynamische Differenzkalorimetrie, Röntgen-dif- fraktometrie und Dynamische Wassersorption verwendet. Die Unter- suchung von Katalysatoren und Elektroden erfolgt per Rasterelektro- nen-, Licht- und 3D-Mikroskopie mit Auswertealgorithmus, ebenso über elektrische Leitfähigkeit, Röntgenfluoreszenz, Gassorption mit Stickstoff, Kohlenstoffmonoxid und Wasser, Helium-Pyknometrie und Röntgenpulverdiffraktometrie. Wiederum werden der Einfluss von Zeit, Temperatur und Druck im Transferprozess, weiterhin der Einfluss von Mischdauer und Trocknungstemperatur bei Herstellung der Elektroden im Tintenprozess betrachtet. Insbesondere wird dem Aspekt der Reproduzierbarkeit der Elektrodenherstellung sowie der Auswirkung einer Kalandrierung in noch nicht dagewesenem Umfang Rechnung getragen, wobei sich verschiedene Methoden für verschie- dene Fragestellungen als geeignet erweisen. Abschließend erfolgt eine in-situ Charakterisierung per Strom-Spannungs-Kennlinien, Zyklovol- tammetrie und Elektrochemischer Impedanzspektroskopie im H2/N2- Modus. Ein mit veränderter Mikrostruktur erklärbarer Effekt der Kalandrierung auf den Massentransport kann nachgewiesen werden. Während die Erkenntnisse zum Elektrodentransfer gerade zur Kosten- senkung verwendet werden können, liefern die betrachteten Charak- terisierungsmethoden die Möglichkeit zur Quantifizierung von Eigen- schaften, was einen elementaren Beitrag zur Prozessentwicklung wie auch für Grundlagenuntersuchungen darstellt. Das mögliche Optimie- rungspotential hinsichtlich Produkt, Prozess und Kosten stimmt positiv für die Zukunft der Technologie. ii Abstract Before penetration of the mass market significant challenges with respect to infrastructure, technology and cost of fuel cell powertrains have to be mastered. From a process perspective efficient manufac- turing technologies can contribute to this goal. This especially applies to the production of the catalyst coated membrane (CCM) as the heart of polymer electrolyte membrane fuel cells (PEMFC) for auto- motive applications. One possible option for continuous production is the so-called decal process, where anode and cathode electrode are coated via an ink process onto a decal foil and are subsequently transferred onto the polymer electrolyte membrane via hot pressing. The aim of this work is thus a comprehensive analysis of this produc- tion method. Both the process window for the transfer of electrodes from decal foil onto membrane and the effects of the parameters of ink and transfer process on structure and function including process reproducibility shall be investigated. A major component of all those aspects is the selection, implementation and assessment of appropri- ate characterization methods. As for the transfer of electrodes from decal foil onto membrane the three critical components of adhesion between electrode and mem- brane, cohesion of electrodes and adhesion between electrode and decal foil are investigated separately with respect to the influence of time, temperature and pressure. While the former is performed via T- peel testing of the model system membrane / membrane, the latter two are performed using a double cantilever beam test and a shear test, respectively. Transfer trials are used to validate the results. Thus, the fundamental mechanisms can be revealed and the transfer pre- dicted. iii Abstract As for the effect of process parameters on structure and function, membrane, catalyst and electrode are characterized via ex-situ meth- ods and catalyst coated membranes are characterized via in-situ methods in specific fuel cell test stands. For characterization of mem- branes, scanning electron and light microscopy, tensile and trouser tear testing, helium pycnometry, differential scanning calorimetry, X- ray diffraction and dynamic water sorption are used. Characterization of catalysts and electrodes is performed via scanning electron, light and 3D-microscopy, furthermore via electrical conductivity, X-ray fluorescence, gas sorption with nitrogen, carbon monoxide and water, helium pycnometry and X-ray powder diffraction. Again, the influence of time, temperature and pressure during transfer, but also the influence of mixing time and drying temperature during the ink process are investigated. Specifically, the aspects of reproducibility of electrode production as well as the effects of calandering are covered in yet unprecedented extent. Different methods prove to be appropri- ate for different aspects of the problem. Finally, in-situ characteriza- tion via current-voltage characteristics, cyclic voltammetry and elec- trochemical impedance spectroscopy in H2/N2 mode is performed. The effect of calandering on mass transport along with the change in microstructure can be substantiated. While the findings for transfer of electrodes are especially useful towards cost reduction, the examined characterization methods provide the possibility for quantification of properties, which is of essential importance for process development as well as for funda- mental investigations. The existing potential for optimization of product, process and cost gives a positive outlook for the future of this technology. iv Inhaltsverzeichnis Kurzfassung ............................................................................................i
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