Polymer electrolyte membrane and direct methanol fuel cell technology © Woodhead Publishing Limited, 2012 Related titles: Polymer electrolyte membrane and direct methanol fuel cell technology Volume 1: Fundamentals and performance of low temperature fuel cells (ISBN 978-1-84569-773-0) P olymer electrolyte membrane fuel cells (PEMFCs) and direct methanol fuel cells (DMFCs) represent promising low-temperature electrochemical power generation technologies that operate on hydrogen and methanol respectively. These technologies have attracted intense worldwide commercialisation research and development efforts with a large element of these efforts directed at materials developments for fuel cell durability and long term operation. This two volume set presents a comprehensive and detailed review of the fundamentals, performance, and i n situ characterisation of PEMFCs and DMFCs. Volume 1 covers the fundamental science and engineering of these low temperature fuel cells, focusing on understanding and improving performance and operation. Functional materials for energy applications (ISBN 978-0-85709-059-1) Functional materials are a class of advanced energy conversion materials of use in photoelectric, thermoelectric, electrochemical, piezoelectric or electromagnetic applications, such as photovoltaics (PV), hydrogen production and storage, fuel cell systems, and demand-side energy management systems. Global demands for lower cost, higher effi ciency, mass-production and, of course, sustainably sourced materials have coupled with advances in nanotechnology to enable an increasingly important role for functional materials in the sustainable energy mix. This book presents a comprehensive review of the issues, science and development of functional materials in renewable and sustainable energy production and management applications. Advanced membrane technology for sustainable energy and environmental applications (ISBN 978-1-84569-969-7) P rogress in membrane materials, selective membrane design, and computer modelling and simulation have contributed greatly to the application of advanced membranes in conventional and alternative power sectors, as well as to clean industry applications. Research and development of membrane systems continues apace towards the goal of simple, effi cient, and easily integrated systems that offer low-cost, reliable processing and operation. This book presents a comprehensive review of membrane science and technology, focusing on developments and applications in the areas of sustainable energy and clean-industry. 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Please recommend it to your librarian so that everyone in your institution can benefi t from the wealth of content on the site. © Woodhead Publishing Limited, 2012 Woodhead Publishing Series in Energy: Number 31 Polymer electrolyte membrane and direct methanol fuel cell technology Volume 2: I n situ characterization techniques for low temperature fuel cells Edited by Christoph Hartnig and Christina Roth © Woodhead Publishing Limited, 2012 Published by Woodhead Publishing Limited, 80 High Street, Sawston, Cambridge CB22 3HJ, UK www.woodheadpublishing.com www.woodheadpublishingonline.com Woodhead Publishing, 1518 Walnut Street, Suite 1100, Philadelphia, PA 19102-3406, USA Woodhead Publishing India Private Limited, G-2, Vardaan House, 7/28 Ansari Road, Daryaganj, New Delhi – 110002, India www.woodheadpublishingindia.com First published 2012, Woodhead Publishing Limited © Woodhead Publishing Limited, 2012 The authors have asserted their moral rights. 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Typeset by Refi neCatch Limited, Bungay, Suffolk, UK Printed by TJI Digital, Padstow, Cornwall, UK © Woodhead Publishing Limited, 2012 Contents Contributor contact details xi Woodhead Publishing Series in Energy xv Preface xix Part I Advanced characterization techniques for polymer electrolyte membrane and direct methanol fuel cells 1 1 Extended X-ray absorption fi ne structure (EXAFS) technique for low temperature fuel cell catalysts characterization 3 E. PR INCIPI , Sincrotrone Trieste S.C.p.A, Italy 1.1 Introduction 3 1.2 Basic principles and methods 4 1.3 Development of techniques 11 1.4 Application to fuel cell inspection 16 1.5 Advantages and limitations 21 1.6 Future trends 22 1.7 Sources of further information 23 1.8 References 23 2 Advanced microscopy techniques for the characterization of polymer electrolyte membrane fuel cell components 26 H. S CHULENBURG , Paul Scherrer Institut (PSI), Switzerland, C. RO TH , Technische Universität Darmstadt, Germany and Karlsruhe Institute of Technology, Germany and F. SC HEIBA , IFW Dresden, Germany 2.1 Analytical challenges in fuel cell research 26 2.2 Imaging of the ionomer 27 2.3 Imaging of electrode porosity 38 2.4 Imaging of the interface between electrode and gas diffusion layer 47 v © Woodhead Publishing Limited, 2012 vi Contents 2.5 The future of advanced microscopy in fuel cell research 53 2.6 Acknowledgements 60 2.7 References 60 3 Differential electrochemical mass spectrometry (DEMS) technique for direct alcohol fuel cell characterization 65 C. C REMERS and D. B AYER , Fraunhofer Institute for Chemical Technology, Germany 3.1 Introduction 65 3.2 Basic principles, cell design and applications 66 3.3 Experimental techniques 73 3.4 Application with respect to fuel cell catalysis 75 3.5 Advantages and limitations of differential electrochemical mass spectrometry (DEMS) 81 3.6 Fuel cell DEMS and in-line mass spectrometry 81 3.7 References 83 4 Small angle X-ray scattering (SAXS) techniques for polymer electrolyte membrane fuel cell characterization 87 X. TU AEV and P. S TRASSER , Technical University Berlin, Germany 4.1 Introduction 87 4.2 Principles and methods of small angle X-ray scattering (SAXS) 88 4.3 Application of SAXS to fuel cell component characterization 102 4.4 Future trends in SAXS-based fuel cell catalysis research 112 4.5 Sources of further information 112 4.6 References 113 5 X-ray absorption near edge structure (∆μ XANES) techniques for low temperature fuel cell characterization 120 D. E. R AMAKER , George Washington University, USA and C. RO TH , Technische Universität Darmstadt, Germany and Karlsruhe Institute of Technology, Germany 5.1 Introduction 120 5.2 Basic principles, methods and theoretical calculations 122 5.3 Applications 129 5.4 Advantages, limitations and future trends 138 5.5 References 141 © Woodhead Publishing Limited, 2012 Contents vii Part II Characterization of water and fuel management in polymer electrolyte membrane and direct methanol fuel cells 147 6 Characterization and modeling of interfaces in polymer electrolyte membrane fuel cells 149 T. SW AMY , The Pennsylvania State University, USA and E. C. K UMBUR , Drexel University, USA 6.1 Introduction 149 6.2 Characterization of interfacial morphology in polymer electrolyte fuel cells (PEFCs) 150 6.3 Experimental investigation of interfaces in PEFCs 159 6.4 Modeling of interfaces in PEFCs 169 6.5 Future work 184 6.6 References 185 7 Neutron radiography for high-resolution studies in low temperature fuel cells 188 D. S. H USSEY and D. L. J ACOBSON , National Institute of Standards and Technology, USA 7.1 Introduction 188 7.2 Experimental layout of a high-resolution neutron imaging beamline 190 7.3 Image acquisition and analysis 195 7.4 Review of recent experiments 205 7.5 Outlook and conclusions 209 7.6 Note 210 7.7 References 210 8 Neutron radiography for the investigation of reaction patterns in direct methanol fuel cells 214 K. WI PPERMANN and A. S CHRÖDER , Forschungszentrum Jülich GmbH, Germany 8.1 Introduction 214 8.2 Principle of neutron radiography imaging 217 8.3 Development of combined high-resolution neutron radiography and local current distribution measurements 218 8.4 Combined neutron radiography and local current distribution measurements 225 8.5 Conclusions and future trends 236 8.6 Sources of further information 239 8.7 References 239 © Woodhead Publishing Limited, 2012 viii Contents 9 Neutron tomography for polymer electrolyte membrane fuel cell characterization 243 I. M ANKE and N. K ARDJILOV , Helmholtz Centre Berlin for Materials and Energy, Germany and C. HA RTNIG , Chemetall GmbH, Germany 9.1 Introduction 243 9.2 Complementarity of neutrons and X-rays 244 9.3 Principles of neutron tomography 246 9.4 Limitations and artifacts 250 9.5 Examples of applications 252 9.6 Outlook 259 9.7 References 259 10 Magnetic resonance imaging (MRI) techniques for polymer electrolyte membrane and direct alcohol fuel cell characterization 262 K. W. F EINDEL , National Research Council Canada, Canada 10.1 Introduction 262 10.2 Concepts of nuclear magnetic resonance (NMR) 263 10.3 Introduction to magnetic resonance imaging (MRI) 269 10.4 NMR and MRI hardware 275 10.5 MRI technical considerations 277 10.6 Adaptation of polymer electrolyte membrane fuel cell (PEMFC) design and materials 282 10.7 Quantifi cation of water content 286 10.8 General water distribution 289 10.9 Water in the PEM 290 10.10 Flow channels 303 10.11 Hydrogen–deuterium contrast 306 10.12 Application to direct alcohol fuel cells 310 10.13 Advantages and limitations 313 10.14 Future trends 314 10.15 Sources of further information 315 10.16 References 315 11 Raman spectroscopy for polymer electrolyte membrane fuel cell characterization 321 H. B ETTERMANN and P. F ISCHER , Heinrich-Heine-University of Düsseldorf, Germany 11.1 Introduction 321 11.2 Raman fundamentals 323 11.3 Experimental setup 328 11.4 Raman spectroscopic investigations on polymer electrolyte membrane (PEM) fuel cells 334 11.5 Outlook and future prospects 346 © Woodhead Publishing Limited, 2012 Contents ix 11.6 Acknowledgments 347 11.7 References 347 Part III Locally resolved methods for polymer electrolyte membrane and direct methanol fuel cell characterization 351 12 Submillimeter resolved transient techniques for polymer electrolyte membrane fuel cell characterization: local i n situ diagnostics for channel and land areas 353 I. A. S CHNEIDER , M. H. B AYER and S. von D AHLEN , Paul Scherrer Institut (PSI), Switzerland 12.1 Spatially resolved characterization of polymer electrolyte fuel cells (PEFCs) 353 12.2 Approaches for the evaluation of the lateral current distribution in PEFCs 355 12.3 Submillimeter-resolved local current measurement in channel and land areas 361 12.4 Local transient techniques in channel and land areas 363 12.5 Combined use of local transient techniques and neutron radiography 374 12.6 Start/stop phenomena in channel and land areas 382 12.7 Concluding remarks 390 12.8 Acknowledgments 391 12.9 References 391 13 Scanning electrochemical microscopy (SECM) in proton exchange membrane fuel cell research and development 399 W. S CHUHMANN , Ruhr-Universität Bochum, Germany and M. B RON , Martin-Luther-Universität Halle-Wittenberg, Germany 13.1 Introduction 399 13.2 Basics of scanning electrochemical microscopy (SECM) 400 13.3 SECM in fuel cell catalyst development and investigation 405 13.4 Towards the characterization of fuel cell electrodes with SECM 418 13.5 Future trends 419 13.6 References 419 14 Laser-optical methods for transport studies in low temperature fuel cells 425 R. LI NDKEN and S. B URGMANN , Zentrum für Brennstoffzellen Technik ZBT GmbH, Germany 14.1 Introduction 425 © Woodhead Publishing Limited, 2012