The Electrochemistry of Solid Oxide Fuel Cell Anodes: Experiments, Modeling, and Simulations
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- Stanislaus Müller
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1 Diss. ETH No The Electrochemistry of Solid Oxide Fuel Cell Anodes: Experiments, Modeling, and Simulations A dissertation submitted to the SWISS FEDERAL INSTITUTE OF TECHNOLOGY ZÜRICH for the degree of Doctor of Technical Sciences presented by Anja Bieberle Dipl.-Ing. Univ. born on October 18, 1971 Germany accepted on the recommendation of Prof. Dr. L.J. Gauckler, examiner Prof. Dr. S. Virtanen, co-examiner Dr. K. Honegger, co-examiner Zürich, 2000
2 1 Summary Summary The electrochemically active component of a solid oxide fuel cell (SOFC) system is the fuel cell itself. It consists of three main parts: the anode, the electrolyte, and the cathode. At the anode the fuel is oxidized and electrons for the electrical current are extracted. Even though the anode is a central part of the SOFC, its electrochemistry is not yet well understood. This is mainly due to three reasons. First, the state-of-the-art cermet anode made of nickel and yttria stabilized zirconia, i.e. Ni-YSZ, has a complex microstructure with three interpenetrating networks of Ni, YSZ, and pores. Thus, it is difficult to characterize and to quantify the area where the electrochemistry takes place. Second, the results obtained from the main characterization method, i.e. electrochemical impedance spectroscopy (EIS), are difficult to interpret in a physical and in a chemical way. Third, fundamental surface science data under the particular operating conditions of SOFCs is not available from the literature. Despite these problems, it is the main goal of this thesis to investigate the anodic reaction mechanisms and to contribute to a better understanding of the electrochemistry of SOFC anodes. In order to reach this goal, a new approach, the so-called state-space modeling (SSM) approach, is used. It combines experiments, modeling, and simulations. The experimental part focuses mainly on EIS measurements of SOFC anodes. Modeling implies that an electrochemical model is established which allows the calculation of impedance spectra directly from the chemical and the electrochemical equations. Hence, the experimentally measured and the simulated impedance data can be directly compared. Equivalent circuit fitting which is conventionally used for the interpretation of EIS data, is not necessary. The approach is described in a general way in chapter 2. Chapter 3 and 4 focus on the experiments of Ni pattern and Ni-YSZ cermet anodes, respectively. Chapter 5 considers the modeling and the simulations in more detail. The electrochemistry of Ni pattern anodes is the subject of chapter 3. By means of this simplified anodic system, the electrochemistry is studied experimentally as a function of several important parameters, i.e. the triple phase boundary (TPB) length, the temperature, the partial pressures of hydrogen and of water, and the overpotential. It is found that Ni pattern anodes are dominated by one main electrode process which might be attributed to the adsorption / desorption of hydrogen or to the removal of oxygen from the electrolyte including charge transfer. A detailed mechanism for the catalytic effect of water on the anode ki-
3 Summary 2 netics is proposed. This simplified anode design emerged to be suitable for a detailed investigation of the electrochemistry of SOFC anodes. Further insight into the electrochemistry of SOFC anodes from an experimental point of view is given in chapter 4: different anode designs are characterized concerning their microstructure and their electrochemistry. The impedance analyses agree with the findings and the interpretations of the Ni pattern anodes. Due to the more complex microstructures of the anodes in chapter 4, further effects and tendencies can be pointed out and the proposed reaction mechanism from chapter 3 is refined. Thus, all the experimental results of the thesis manifest that Ni-YSZ SOFC anodes are limited by two main processes, i.e. the adsorption / desorption of hydrogen including charge transfer and the desorption of water. Modeling and simulations are finally merged in chapter 5 with respect to the simplified anodic SOFC system Ni, H 2 -H 2 O YSZ. An electrochemical model is established using literature data as far as available. The simulations are based on this electrochemical model. The comparison of the simulated and the experimental impedance spectra show a rather good coincidence of the data. The behavior of the simulated spectra under parameter variations similar to those carried out in the experiments on Ni pattern anodes confirm that the established electrochemical model is appropriate. However, on the basis of the impedance results and interpretations of the experimental work, modifications of the electrochemical model are recommended for the future. Summarizing, it can be stated that the state-space modeling approach combining experiments, modeling, and simulations, has emerged as an extremely promising method to investigate the electrochemical behavior of SOFC anodes. The results obtained in this thesis contribute significantly to a better understanding of the electrochemistry of SOFC anodes.
4 3 Zusammenfassung Zusammenfassung Der elektrochemisch aktive Teil eines Festelektrolyt-Brennstoffzellen (SOFC) Systems ist die Brennstoffzelle selbst. Sie besteht aus drei wichtigen Bestandteilen: der Anode, dem Elektrolyt und der Kathode. An der Anode wird der Brennstoff oxidiert und die Elektronen für den elektrischen Strom erzeugt. Obwohl die Anode eine zentrale Rolle spielt, ist die zugrundeliegende Elektrochemie bis heute nicht zufriedenstellend verstanden. Das ist hauptsächlich auf drei Gründe zurückzuführen. Erstens haben die heutzutage verwendeten Cermet-Anoden aus Nickel und Yttriumoxid stabilisiertem Zirkonoxid (Ni-YSZ) eine komplizierte Mikrostruktur, die aus drei ineinandergreifenden Netzwerken aus Ni, YSZ und Poren besteht. Es ist daher schwierig, den elektrochemisch aktiven Teil der Anode zu charakterisieren und zu quantifizieren. Zweitens können die Ergebnisse, die von der wichtigsten Charakterisierungsmethode der Anoden, der elektrochemischen Impedanzspektroskopie (EIS), erhalten werden, nur schwer in physikalischem und chemischem Sinne interpretiert werden. Drittens fehlen grundlegende Daten aus der Literatur der Oberflächenforschung, die das System unter SOFC Betriebsbedingungen charakterisieren. Trotz dieser Probleme ist es das Hauptziel dieser Arbeit, die Prozesse, die an der Anode ablaufen, zu erforschen und zu einem besseren Verständnis der Elektrochemie von SOFC Anoden beizutragen. Um dieses Ziel zu erreichen, wurde ein neuer Lösungsansatz verfolgt, der auf einem sogenannten Zustandsraummodell (SSM) beruht. Er verknüpft Experimente, Modellierung und Simulationen. Von der experimentellen Seite her werden hauptsächlich EIS Messungen von SOFC Anoden durchgeführt. Bei der Modellierung wird ein elektrochemisches Modell aufgestellt, das es ermöglicht, Impedanzspektren direkt von den chemischen und elektrochemischen Gleichungen zu simulieren. Die experimentellen und die simulierten Impedanzspektren können direkt miteinander verglichen werden. Die konventionelle Methode EIS Daten zu interpretieren, nämlich das Fitten mit äquivalenten Schaltkreisen, ist nicht notwendig. Der neue Lösungsansatz ist allgemein in Kapitel 2 beschrieben. Die Kapitel 3 und 4 konzentrieren sich jeweils auf Experimente an mikrostrukturierten Ni und Ni-YSZ Cermet-Anoden. Das Kapitel 5 behandelt die Modellierung und die Simulationen. Die Elektrochemie von mikrostrukturierten Ni Anoden steht im Fokus von Kapitel 3. Anhand dieses vereinfachten anodischen Systems wurde die Elektro-
5 Zusammenfassung 4 chemie experimentell als Funktion von den folgenden Parametern untersucht: der Länge der Dreiphasengrenze (TPB), der Temperatur, dem Partialdruck von Wasserstoff und Wasser und der Überspannung. Man fand, dass mikrostrukturierte Ni Anoden hauptsächlich von einem Elektrodenprozess bestimmt werden. Dieser Prozess kann entweder der Adsorption / Desorption von Wasserstoff oder dem Ausbau von Sauerstoff aus dem Elektrolyten mit gleichzeitigem Ladungstransfer zugeschrieben werden. Für den katalytischen Effekt von Wasser auf die Kinetik wird ein ausführlicher Mechanismus vorgeschlagen. Die Untersuchungen an dem vereinfachten Anodendesign haben sich demnach als geeignet für die Erforschung der Elektrochemie von SOFC Anoden herausgestellt. Weitere Einblicke von experimenteller Seite werden im Kapitel 4 gewährt. Verschiedene Anodendesigns wurden bezüglich ihrer Mikrostruktur und der Elektrochemie charakterisiert. Die Analyse der Impedanzdaten stimmt mit den Ergebnissen und den Interpretationen der mikrostrukturierten Ni Anoden überein. Aufgrund der komplexeren Mikrostrukturen der Anoden in Kapitel 4 konnten weitere Effekte und Tendenzen verdeutlicht und der vorgeschlagene Reaktionsmechanismus von Kapitel 3 verfeinert werden. Alle experimentellen Ergebnisse der Arbeit verdeutlichen nun, dass Ni-YSZ SOFC Anoden durch zwei Prozesse limitiert werden: die Adsorption / Desorption von Wasserstoff mit gleichzeitigem Ladungstransfer und die Desorption von Wasser. Die Modellierung und die Simulationen werden schliesslich in Kapitel 5 anhand des vereinfachten anodischen Systems Ni, H 2 -H 2 O YSZ behandelt. Ein elektrochemisches Modell wurde mit Hilfe der Literatur aufgestellt. Die Simulationen stützen sich direkt auf dieses Modell. Ein Vergleich der simulierten und der experimentellen Impedanzspektren zeigte eine ziemlich gute Übereinstimmung der Daten. Das Verhalten der Spektren, die unter den gleichen Bedingungen simuliert wurden wie die Experimente an den mikrostrukturierten Ni Anoden durchgeführt wurden, bestätigte, dass das aufgestellte elektrochemische Modell die experimentellen Daten ziemlich gut darstellt. Jedoch wird aufgrund der EIS Daten und der Interpretationen der experimentellen Arbeit empfohlen, in der Zukunft Modifikationen des elektrochemischen Modells vorzunehmen. Zusammenfassend kann man festgehalten, dass der Ansatz der Zustandsraummodellierung, welcher Experimente, Modellierung und Simulationen vereinigt, eine sehr vielversprechende Methode ist, um die Elektrochemie von SOFC Anoden zu erforschen. Die Ergebnisse dieser Arbeit tragen eindeutig zu einem besseren Verständnis der Elektrochemie von SOFC Anoden bei.
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